FI101087B - Method for Controlling Thermosetting and Synthetic Fiber Manufacturing Processes of Synthetic Fiber Gums for the Production of Nonwoven Fabrics with Desired Strength Properties - Google Patents

Abstract

A regulation method for regulating the thermobonding processes of synthetic fibre webs and the production processes of synthetic fibres for the preparation of nonwoven fibre fabrics having the desired strength properties. In the method according to the invention, fibres are made from a polymer, especially a polyolefin polymer, using melt spinning methods, and from these fibres, fibre fabric is made using thermal bonding methods. The central processing conditions of both the fibre and the fabric are adapted using the regulation method according to the invention and associated regulation model so that as a result of thermobonding, the desired nonwoven fabric is obtained having regulated strength properties.

Description

101087

Method for Controlling Thermosetting and Synthetic Fiber Manufacturing Processes of Synthetic Fibers for Nonwoven Nonwovens with Desired Strength Properties 5

In the process according to the new invention, fibers are produced from a polymer, in particular polyolefin polymers, using melt-spinning methods and from these fibers using thermal bonding methods using a nonwoven fabric. The main processing conditions for the production of both fiber and fabric are adapted using the control method according to the invention and the related control model, so that thermosetting results in a controlled nonwoven fabric with strength properties. The control method according to the invention is an empirical method simulating test results guaranteeing both pilot and production dimensions and based on these results and the observations made, for which there are also basic scientific • | 20 roads.

In the control method according to the invention, the characteristic features set by the control bases and their fiber production and thermobonding processes include:; 25 - The control method is designed for the direct control of production processes, but it can also be used quite well in product development and corresponding test runs.

101087 2 - The framework of the control method is a dynamic control equation of the form φ = v'n x expf-aj λ] x cx x T2 x exp [-E / RT] 5 = v "nx exp [-a2 fav] x c2 x T2 x exp [ -E / RT] = cx T2 x exp [-E / RT], where φ is the strength property of the fabric: longitudinal or transverse tensile strength, elongation or breaking 10 v is the velocity of the gauze web in relation to the heating rate of the gauze λ the average chain orientation of the fiber structure T is the temperature (usually the pin-15 temperature of the smooth bonding roll) E is the activation energy a and c of the bonding process are constant - The control function φ is increasing as a function of temperature, but at 20 the point of intersection is the maximum value of the control strength and the corresponding temperature.It should be noted that this value of the maximum strength corresponds to • 25 most often the results of the measurement. values.

- The variable and parameters corresponding to the control equations are determined in roller bonding with fiber-specific pilot tests 101087 3 and in air and furnace bonding either by thermomechanical Lenk tests or also by pilot tests.

- The values of maximum strength and corresponding temperature according to the control equations are each a function of the crystalline lamellar thickness of the polymer structure of the spun fiber, in the form (e.g. with respect to tensile strength): σ, ^ = c3 Dz ~ nl and = T - c4 Dz_1, where Dz is (Lorenz-corrected) ) crystalline lamellar thickness.

10 In the control method, the crystalline lamellar thickness is determined as the product of the long period obtained from low-angle X-ray scattering (Lorenz-corrected) and the degree of crystallinity obtained from wide-angle scattering. It should be mentioned that the melting point (partial melting) of the crystal regions of the polymer is linear with respect to the inverse of the crystalline lamellar thickness, so the dependence between the above-mentioned maximum value of the bonding temperature and the lamellar thickness can be elucidated naturally. It should be noted that according to the equations, the increase in lamella thickness has an upward effect on the temperature values and a decreasing effect on the maximum strength values.

- In the control method, the fiber production is controlled by adjusting the crystalline lamella thickness of the spinning fiber, which is performed with respect to the degree of crystallinity by turning off the spinning fiber. 25 by adjusting the speed and temperature of the reaction and by adjusting the extinguishing rate and temperature for a long period of time, as well as the degree of the chain length of the polymer and, for example, the isotacticity of the propylene polymer.

101087 4 - The orientation of the spinning fiber and the strength values of the thermal bond, respectively, are also controlled by adjusting the tension of the fiber cable in the spinning.

5 - By adjusting the temperature difference of the binding rolls, the strength properties of the product fabrics can be fine-tuned in the opposite direction with respect to the binding equation. The control method is based on the change in both fiber deformation and heat transfer.

10 - The temperature dependences of the bonding equations corresponding to the longitudinal and transverse tensile strength values of the fabrics are usually the same. The elongation values of fabrics are quite susceptible to external influences (temperature, types of radiation, etc.), so the corresponding lubrication energies of the equations Akti-15 often differ from the energy values of the tensile strength equations. Especially at high temperatures, above the temperatures corresponding to the maximum values of the strength values, a large dispersion of the activation energy values per fiber can be observed. This usually requires fiber-specific determination of these 20 energy values over the entire temperature range. The decrease in strength values at high temperatures is due to fiber deformation, chain degradation caused by autogenous oxidation, and fiber clogging. The variation in the number of partial fuses also causes scattering at 25 energy values.

- Guided by the control equations, the values of the thermal strength product strengths can be adjusted over a wide range as a function of the gauze web speed, the bonding temperature and the fiber draw ratio.

101087 5

At the ratios of the strength values of the product fabrics, the temperature dependences are often not equal. This must be taken into account, in particular, when requirements are laid down for the strength-5 of the final products in terms of the relationships between or between longitudinal and transverse strength values.

In this case, several paths lead to the required result, and the path of the "lowest damage" must then be searched for by the control computers of the equipment or determined in advance for each fiber by means of a map prepared using control equations.

- The control and regulation equation for fabric production can also be constructed synthetically using observations of the dependence of the maximum strength and the corresponding temperature on the crystalline lamella thickness of the fiber polymer. The web speed exponent of the weather equation and the constant coefficient of the draw ratio have low limits of variation and are close to one, so empirical coefficients can be used. The values of the activation energy of the binding are almost the same in stable nonwovens (E ~ 40 kcal / mol). By placing these values in the control equation, an estimate of the equation is obtained, which can be used in product development and in the control of parameter measurement times.

25 - The control equation 101087 6, which is well considered, is suitable for adjusting the strength properties of thermosetting product fabrics formed by nested coke component fibers of different quality or of the same quality. In this case, the crystalline lamellar thickness of the fiber polymer corresponds to the structure of the shell layer. In the manufacture of skin-core structured fibers (nested nozzle spinning, peripheral oxidation, etc.), the chain distribution-5 ma values of the polymers, the viscosity values of the melts, the temperatures of the spinning melts and the spinning draw ratio play a role. These act as either parameters or variables in thermal bonding control. The magnitude of the apparent activation energy values of the thermal bonding of the nested fibers is a function of the spinning treatment and is susceptible to decomposition due to the (large) number of total or partial melts. Determining the coefficients of the thermobond control equation for bicomponent fibers is not easily possible without accurate pilot measurements.

When carrying out the control method according to the invention, it must be taken into account that in the production and thermal bonding of fibers often include fiber polymer grades, spinning and bonding capacities, fabric weights, distribution of "bonding points" subject. When developing the control method for thermal bonding, these variables have been considered as parameters, the effect of which on the control equation must always be determined experimentally when changes occur.

25

The new control method according to the invention is described by the first claim, the content of which is also in the review.

101087 7

There are many points of connection to the control method under consideration in the rather extensive patent and technical literature on thermal bonding.

5 Only a very limited number of publications can be considered in this context. These usually have a very large number of patent and other referenced publications. There are separate issues related to the control method according to the invention in almost all thermal bonding and fiber production methods utilizing synthetic and natural fibers.

A brief review of technical scientific publications and bonding models related to thermobonding technology, as well as 15 patent publications.

In his series of publications (1994-95), Alfred Watzl / 1 / gives a very good and detailed description of the theoretical foundations of current non-woven technology, practical experiences and market developments.

S. B. Warner / 2 / shows different thermomechanical processes of thermobonding and gives an estimate of the effect of each process on thermobonding. The publication states • the limited nature of the conductive heat transfer of thermal bonding and the importance of the line-facilitated flow in the heat transfer. The proportion of deformation heating (ca. 2G-35 ° C) caused by roller bonding in the gauze in the bonding is small but important. Examination of the effect of Clapeyron 101087 8 shows only a limited amount of melting (effect n.

10 ° C) under high pressure. The effect of diffusion on the mass transfer of the binding is not important: a diffusion distance (including other effects) of a gyration radius (~ 500 Å) requires a delay time of about 1-2 seconds, while the delay time of the "gauze bond" in the roll interval is of the order of only 10 ms. In the bonding periphery, the thermomechanical and as yet uncontrolled thermomechanical history of the polymer also limits product strength.

In the thermal bonding process, D. Muller / 3 / has studied in particular the role of roller pressure in heat conduction, the effect of production rate, temperature, pressure and bonding pattern on the bonding process. D. Möller / 3 / and S. Klöcker 15/3, 4 / have developed a process model suitable for nonwoven thermal bonding. The model makes it possible to describe the deformation properties of nonwoven under processing conditions between bonding rollers. The model allows the correlation of fiber material properties to process parameters. The material model of the model 20 is Zerner's 3 p solids model, which includes, in addition to temperature and pressure, the elasticity and damping characteristics of the material. The properties of the fibrous material are easily obtained from elasticity and relaxation measurements. In the region of melting of the polymer 25, the elastic characteristic is significantly reduced, because in the roll space part of the volume loses its elastic properties. In short, in the model, partial melting is obvious and is adopted as such (parameter), the bond strength is a function of the line pressure of the rolls, and the line pressure substantially improves the conductive heat transfer.

The measurement results show that with the given fiber material and unit weight, the production rate, the required Vals-5 blade pressure and finally the roll geometry can be predicted even more accurately. Further, the mechanical deformation properties of the nonwoven described by the model can be combined with the roll deflection compensation calculations and the control system.

10 T.F. Gilmore et al. / 5, 6 / examine the strength properties of point-bonded products using both our own and literature research and thermosetting models. According to the review, 15 factors related to thermobonding (1993) include: the effect of fiber elongation, the effect of the thermal history of the fibers, and the effect of the basic properties of the fibers on the bond strength; the effect of temperature on the bonding properties and the morphology of the bulk polymer in the bond is unknown; The effects of the Clapeyron effect, the shape of the binding point-20, and the distribution of batteries are unexplained; the effect of the temperature difference of the binding rollers is not known; the effect of the cooling rate on the product is unknown, - the reasons for the difference in the longitudinal and transverse properties of the fabrics have not been elucidated, etc.

25 T.G. In a computer model based on the Box-Hunter model (/ 6 /, 1994), in addition to regression coefficients, Gilmore uses four process variables (roll temperature, load, line speed, and gauze weight) to evaluate the physical properties of the thermosetting product. The evaluation of the results states that the method is useful in the optimization of thermobonding processes and in the elucidation of the mechanism. The most important result is that almost all product properties correlate strongly with the bonding temperature, with other factors being of lesser importance.

Let us briefly consider the two computer models used for the study of the spunbonding process, both of which focus on the pre-spinning fiber-10 spinning process.

S. Misra et al. / 7 / apply a mathematical model of the spinning process to study the effect of various process and polymer variables on the structure and properties of product filaments. The material parameters studied 15 were elongational v. And kinetics of pressure-induced crystallization. Variable parameters included extrusion temperature, cable line length (SL), temperature, cooling air flow rate, draw-down venturi shape, and nozzle capacity. The model shows that tensile-20 viscosity is a key factor in controlling draw-down rate, crystallization temperature, and orientation development in the fiber. Among the process parameters, the cooling air temperature and flow rate have the greatest effect.

A.C. Smith et al. / 8 / have prepared a model for fiber formation in the spinning-25 tap process. The model equations include the Ziabick crystallization rate equation as well as the empirical crystallization rate pressure effect parameter. The models enable e.g. an estimate of the onset and position of crystallization 101087 11 advancing along the spinning line. The computer results and the experimental results are consistent.

The level of thermal bonding of polypropylene, polyester and bicomponent fibers should be mentioned without reference to some publications / 9 /.

It should also be mentioned that R.J. Kerekes / 10 / has developed a basic model for the heat transfer of calenders, which is referenced by many researchers in coriander mosidation.

Finally, let us briefly look at the state of the art in thermal bonding with the help of some patent publications. The patent publications mainly deal with spinning, as this si-15 contains essential factors affecting thermal bonding in terms of both fiber production and bonding.

R.V. Schwartz (/ 11 /: US 4,100,319 / 1978) performs the production of high-spinning fiber gauze (as in U.S. Pat. No. 3,855,046) and direct thermal bonding of the gauze (as opposed to U.S. Pat. No. 3,692,618) without preheating. The method believes that the gauze filament must not exceed a certain low level of crystallinity prior to bond formation, so rapid heating of the gauze is necessary. In order to clarify the corresponding state of the art, the • method.

25 patents mention 12 patented methods / 11 /.

The patent for the manufacture and bonding of peripherally oxidized fiber (/ 12 /: US 5,282,378 / 1994) discloses the oxidation of a polymer having a high melting temperature, spinning 101 '12 ϋ, ίϋι-spun and "high" MWD dispersion to a skin-core structured fiber, with good thermosetting properties. 76 publications (including 50 US-5 patents) are described in the description of the prior art of the patent publication. The 'Finnish' patent applications FIA 943072 / 23.06.94 and FIA 942889 / 16.06.94 also apply to the same peripheral oxidation.

A limited review of 10 publications related to thermal bonding technology did not reveal a comprehensive, "temperature-controlled" method or control model comparable to the new thermal bonding control method. In several publications, temperature was found to be relevant to the formation of relevant bond strength in addition to pressure.

The operating principles of the new thermal bonding control method are described in detail in the following examples.

20 25 101087 13

Example 1.

Example 1 shows, by means of detailed examples, the basics of the new invention and the related essential findings.

Sub-Example 1.l

Sub-Example 1.1 demonstrates the manufacturing equipment and functions of the fibers and fabrics used in the process development corresponding to the Example 10 portion of the Invention.

In the preparation of the fiber-15 sample sets appearing in the method description of the new invention, both the so-called short-spinning and high-speed spinning methods and similar equipment. The following terms are used in this review: short and quick spinning method.

Spinning and tensile test series were mostly performed on pilot 20 scale equipment, which differed from production scale equipment only in the number of spinning units, but not in size. The pilot equipment was better equipped in terms of measurement technology than the production equipment.

«25 The number of nozzles in the nozzle plate conventionally used in short-spinning equipment was 30,500 and the diameter of the nozzles was 0.25 mm. In this case, the capacity of the equipment (P, kgh’1) was a function of □ Γι as a function of the polymer pump speed (nr, min’1).

101 14 Ρ = 2.0437 χ no / 1 /

The speed of the polymer in said nozzle (vs / m min "1) was vg = 2.5111 χ ΙΟ'2 x nr / 2/5. In the speed range nr = 15-20 of the polymer pump, the magnitude of the capacities and nozzle speeds of the equipment is given: P = 31-41 kgh'1 and vs = 0.38-0.50 m min'1 The number of nozzles and in particular the diameter could be varied if necessary by changing the nozzle plates.

10 The quick-spinning machine had two parallel nozzle plates, a total of 1,200 nozzles and a flow-shaped nozzle outlet diameter of 0.4 mm. The capacities of the fast and short spinning machines were the same, but their 1-gallet speeds had a difference of about ten times (about 1000 and 100 m min’1). There was a considerable difference in the cooling systems of the spinning fibers of the spinning methods: the length of the cooling zone (gap) of the fast spinning method was about 2 m and that of the short spinning method about 50 mm, respectively. The fast spinning methods have 20 efficient fiber cooling air cooling equipment as well as easily adjustable and uniform fiber-specific cooling, which are difficult to implement in the short spinning methods. The sub-assemblies of the short-spinning traction equipment, Fig. 1, are: 1. extruder, 2. melt-spinning equipment, 3. l-galetisto, 4. ve-25 furnace, 5. 2-galetisto, 6. 2-avivivo, 7. curler, 8. stabilization and drying oven and 9th staple fiber cutter. The hardware diagram of the quick spinning method is essentially analogous to the diagram of Figure 1.

101087 15

Some of the fiber sets of the examples were manufactured with production-guaranteed short-spinning drawing equipment. In some fabric fabrication experiments, fibers made by rapid spinning methods were used. Some of the samples used to elucidate the details of the invention were prepared under controlled conditions with a Haake-Rheocord-90 apparatus, which was also equipped with a mechanical traction apparatus with ovens.

10 A diagram of a conventional apparatus used in the manufacture and bonding of fibrous gauze is shown in Figure 2. The parts of the equipment are: 1. opener, 2. fine opener, 3. charge silo, 4. feeder, 5. card, 6. binding rollers and 7. reel machine.

15 The equipment in the diagram is all production scale. The fabrication and binding speed of the binding line gauze web were adjustable in the speed range of 25-100 m min. "1. The upper roller of the diamond or round embossed binding device and the smooth lower roller were temperature and pressure adjustable. The binding rollers had a production scale of only 2.2, but their width was only wide. m.

In the studies of the fiber binding mechanism, the so-called fiber loop bonding and direct bonding tests with a mechanical J 25 and a dynamic mechanical thermal analyzer (Mettler 3000 / TMA 40 and Seiko 5600 / DMS-200 analyzer).

101087 16

Sub-example 1.2

Sub-Example 1.2 considers the rate of change in the long identity period of a fiber polymer (here polypropylene) as well as the degree of crystallinity as a function of temperature and time.

From the value of a long identity period (statistical), the value of the degree of crystallinity can be used to calculate e.g. the statistical value of the crystalline (as well as amorphous) layer thickness of the polymer as a function of time and temperature.

10

For all test polymers, the same long-term values as a function of temperature and time (regardless of different polymer starting values) were obtained in the measuring range, within the limits of measurement accuracy, which contributes to the independence of 15 periods from the degree of crystallinity.

The structural system of the considered propylene polymer has a Lorenz-corrected long period (Lz, Ä) value as a function of temperature (T, K) and time (t, min) of the form 20 Lz = 92.64 + 1864.4 / (435.44-T) + [ (465.0 / (444.01-T)) - 3.7326] In t / 3 /

The following equations are obtained for the differential changes of the period as a function of temperature and time

Lz / dT = 1864.4 / (435.44-T) 2 + [465.0 / (444.01-T) 2] In t / 4/25 Lz / dT = [(465.0 / (444, 01-T)) - 3.7376] t'1 / 5 /

From the equations, it can be stated that the long-term time dependence is also a function of temperature. The value of Pit.Τ ·] 101Γ 17 for a long period increases strongly as a function of temperature, especially as the melting point of the polymer approaches.

Since the long identity period (L *, Ä) is the sum of the amorphous and crystalline lamellar thicknesses of the polymer 5, the crystalline lamellar thickness (D *, Ä) is obtained by fc x L *, where fc is the crystallinity degree fraction. The Lorenz-corrected measurement value of the period (Lz, Ä) is used in this review. There is an approximately linear relationship between the period values, which in the experimental series was of the form L * = 1.064 x Lz + 30.59 / 6 / When implementing the control method, the absolute value of a long identity period is not necessary, especially when the difference in values is small.

15

Changes in the degree of crystallinity of the fiber polymer in the bond are quite important to the control method, but difficult to determine and estimate because the delay time of the bond is only on the order of milliseconds per bond point.

The change in the degree of crystallinity (fc = χ / 100) of the fiber B1 used in the bonding study (Tables 1 and 2) as a function of time and temperature was monitored after isothermal heat treatment (θ = 80 ° -140 ° C, t = 1-1800 min) with WAXS and With SAXS analysis (devices: Philips PW1730 / PW1710, Kratky).

Taking the ratio ex = χ / X, max as the crystallized fraction of the polymer (B-1: after continuous annealing xmax = 55%), it was found that the increasing crystallinity fraction followed the kinetic equation of Av-ram. The result was the function a for the crystallizing fraction: 101087 18 α = l-exp [-1,8304 χ ΙΟ3 χ exp (-5984,34 / RT) χ t0.075], / 7 / where R, cal / degree-mol is common the gas constant; T, K is abs. temperature and t, min is the time of isothermal crystallization.

The obtained equation simulates well the obtained measurement results. At a temperature of 140 ° C, a slight scattering due to surface melting of the lamellae occurred.

Equation / 7 / has a special low value of the time exponent (n = 0.075) compared to the time exponent of the sample taken directly from the melt state to the isothermal crystallization. The value of the activation energy of the equation (E = -5480 cal / mol) is also lower than the normal value (obtained without correction of the crystallization temperature). These differences are apparently due to the progress of the primary crystallization (during spinning cooling of the sample) with its core formation and growth to such an extent that the values mentioned in the secondary crystallization fall, while maintaining the Avram equation.

The equation form is also well suited for simulating the measurement results of the change in the degree of crystallinity of the fiber polymer B1: 20 χ / 100 = fc = 50.690 exp (-2002.16 / T) + 0.03325 log t / 8 / However, the time exponent of this equation did not remain constant format equation was introduced.

For the fiber polymer A-1 (Table 2) it has a monoclinic starting structure * 25 and a high primary crystallinity degree, i.e. χ = 43.6% (the sample B-1 had a smectic starting structure).

The secondary crystallization of the fiber polymer Al is well simulated by an Avram-type equation, where the time exponent was 101087 corresponding to the previous 19 samples (n = 0.075) and the rate constant in the form k = 6.3088 x 103 exp (-6275.49 / RT) / 9/5 standard values are taken as an example in Table 3.

From equations (3-5) it can be stated that the increase in crystalline lamella thickness is monotonic as a function of temperature.

10 Further from the equations, it can be seen that in the temperature range under consideration, the amorphous lamellar thickness, (l-fc) L2, is characterized by a deep minimum. Thus, the amorphous lamellar thickness initially decreases with increasing temperature and degree of crystallinity (i.e., decreasing amorphous fraction), but then begins to increase strongly after a minimum range in the temperature range of 100 ° -130 ° C. In practice, the crystalline lamella thus increases in length and tapers, whereby the amorphous lamella may increase in thickness, even if the amorphous fraction of the matrix decreases.

The crystalline, as well as amorphous, lamellar thickness of the polymer and its changes can be adjusted quite precisely by adjusting the degree of crystallinity of the polymer matrix and its long identity period. The degree of crystallinity is adjusted in particular by adjusting the temperature of the polymer matrix. Long period adjustment is done by adjusting both the temperature and time of the matrix. The primary magnitude of a long period can be influenced by e.g. weathering and quenching temperature of the spinning polymer at 101087 20 d. The choice of molecular weight and weight distribution of the polymer is important in this context.

The cooling temperature range relevant to the formation of the spinning structure of the fiber polymer is in the range of the maximum crystallization rate temperature (crystallization temperature, where the inverse of the crystallization half-life is maximum), which is determined experimentally (there is also an orientation function). It can be shown (13) that with a maximum crystallization rate of 10 = 90 °, a cooling rate of T90> 80 ° C / s gives the structure a smectic phase in addition to amorphous (α-crystallinity: χ <20%). In the cooling rate range of 20 <T90 <80, the structure has a monoclinic phase in addition to the smectic and amorphous phase (χ: 20-40%) as the cooling rate decreases. As the cooling rate decreases, T90 <20 ° C, the smectic phase is completely lost (χ: 40-60%).

Sub-Example 1.3 20 This sub-example considers the formation of a bonding equation simulating the change in the properties of the product fabrics of the fiber thermal bonding process. The equation is used to * * mainly examine changes in the mechanical strength properties of fabrics as a function of bonding temperature and time.

Thermal bonding of synthetic fibers is a rather complicated event, dominated by different mechanisms in the varying temperature and velocity ranges 101087 21. In this review, an attempt has been made to examine the thermal binding results using two binding equations that simulate these without interfering in detail with the details of the different mass transfer mechanisms.

5 In this review, the tying mechanism as a working hypothesis is divided into three stages:

The first bonding step is the formation of contact points between the fibers of the gauze, apparently as a dislocation-mediated displacement slip. In this case, the effective compression pressure 10 (given by the bonding rollers) at the bonding point is above the yield point of the polymeric material. In practical bonding, this bonding step takes place at an almost momentarily increasing temperature (material constants are a function of temperature; bonding rollers are at high temperature, but the gauze is cold) and stops when the displacement movement is prevented when the compression pressure drops below the yield point.

The second bonding step is assumed to occur as a thermally activated, time-dependent transition creep, which occurs below the yield point of the material. In this case, the displacements circumvent the anti-slip barriers, for example by dislocation-mediated, diffusion-controlled 'snapping'.

In the third bonding step, so much of the melting phase is formed in the partial melting of the polymer that the contact formation takes place by a viscous flow mechanism. In addition to this, other influential phenomena also occur in the system: e.g. diffusion material flow, melting and recrystallization of the fine crystalline portion of the polymer, etc. As the temperature continues to increase, the bond strength begins to decrease due to shrinkage of the bonding fibers, thermal degradation (function of antioxidant quantities and grades), melt overgrowth, etc.

5

Denote the variable characteristic of the fabric (longitudinal and transverse strengths, elongations, toughnesses, etc.) caused by the bonding by the letter φ. The effect of the increase in the contact surface on the variable property gives a temperature-10 activated, dynamic general velocity equation άφ / άΤ = C "x v'1 x kasvη x exp [-E / RT], where / 10 / C" is constant, E is the activation energy, R is general gas constant, T is abs. temperature, v is the heating rate of the fibrous gauze.

15 The integrated form of velocity equation / 10 / is (assuming that 2RT / E << 1) Φ J άφ / φη = C 'x v 1 x T2 x exp [-E / RT] / 11 / Φο. . 20 = C x T2 x exp [-E / RT], where / 12 / n is the exponent dependent on the mass transfer mechanism.

In the third stage of bonding, the equation describing the decrease of strength values is e.g. for analog reasons, also the above-mentioned equation / 10-12 /, which can also be used to simulate changes in the properties corresponding to the aging of the polymer.

The fit of the strength values of the 30 test fabrics prepared on both the pilot and production scale to the bonding equations 101087 23 (on both sides of the maximum values) is quite good (tensile strength and elongation measurements: test strip 5 x 20 cm, tensile speed 30 cm / min; equation: n = 0, φ0 = 0). The heating rate of the fibrous gauze is assumed to be constant as well as a simple 5-fold linear relationship with the web speed of the gauze.

Table 1 summarizes the values of the measurement results obtained in the bonding of different types of test fibers in the form of an equation. The values of the properties of the fiber fibers of the fiber gauze test fibers in the bonding experiments are summarized in Appendix Table 2.

Sub-example 1.4

Sub-Example 1.4 considers the formation of maximum values for the tensile strength (and elongation) of fabrics obtained in the thermoset-15 of test fibers.

In this consideration, the intersection of the bonding equations of the low and high bonding temperature ranges shown in Sub-Example 1.3 is taken as the maximum value of the tensile strength of the thermoset nonwoven fabric. The measured values of the tensile strengths of the test fabrics require the use of two separate equations to describe the bonding process, although there is a transition zone in the immediate vicinity of the intersection points, where the measurement results are slightly below the calculated values. However, this transition range is narrow, especially for conventional fabric strengths, where the change in strength as a function of temperature is lower than for high strength fabrics. The maximum tensile strengths corresponding to the intersection points of the bonding equations are marked in Table 1 in addition to the bonding equations.

The fibers corresponding to the bonding equations have a degree of crystallinity determined as shown in Sub-Example 5 1.2, a Lorenz-corrected long period and a crystalline lamellar thickness. The crystalline lamellar thickness value is indicated for each fiber in Table 1.

Figure 3 shows the above maximum strength values as a function of the crystalline lamella thickness. The logarithmic dependence of the image gives the equation amax = 1192.7 X Dz ’°’ 854/131 /

The scattering of the observation points in the figure is influenced by many factors, such as: - The different tensile ratios of the mechanical fibers following spinning, which are close to the tensile ratio value for structurally homogeneous fibers, λ = 1.0.

- Carding and weight variation of test gauze.

20 - The surface area, shape and distribution of the binding roll on the surface of the roll. The figure shows the transition from one change of pattern roll to another marked with a dashed line (straight H).

- Rate of change of crystallinity and period values as a function of temperature 25.

- Some of the test fibers were imported fibers whose manufacturing conditions are not precisely known (inhomogeneous in cross-section, chain-modified3a, skin-core, spinning, etc. fibers).

101087 25

The temperature corresponding to the maximum tensile strength obtained from the point of intersection of the bonding equations is a function of the inverse of the crystalline lamellar thickness of the fibrous polymer structure of the form 5 Tm = 455.79 - 9.777 X 102 x D, '1/132 /

The dependence according to equation / 132 / has also been found to exist between the melting point of the crystal regions of the polymer matrix and the crystalline lamellar thickness / 14 /, so Equation-10 also has a scientific basis.

In Section Example 1.5, the effect of mechanical tensile ratio on thermal bonding is considered. From the intersections of the bonding equations (Table 3), the equation amax = 45.807 x λ'0'8226 / 14 / is obtained for the dependence between the maximum strength and the tensile ratio (λ = 1.0-2.5).

Thus, the maximum strength of the fabric is equal to the tensile ratio, λ = 1, i.e. when operating with the same polymer and under the same manufacturing conditions, the highest fabric strength is obtained with the spinning fiber, which observation is quite important.

In said test run (1.5), the average chain orientation (fav) of the fiber matrix as a function of the draw ratio was

In λ = 6.6015 fav - 3.6308 / 15/25 i.e. by placing CJmax = 9.078 x 102 exp [-5.4302 fav] / 16 /

Equation / 16 / combines the maximum strength of thermal bonding in question. to the values of the chain orientation of the fiber corresponding to the manufacturing conditions and thus also to the spinning orientation.

101087 26

The maximum strength values of the nonwovens obtained by thermal bonding of the gauze can thus be adjusted by adjusting the crystalline lamella thickness of the spinning fiber. This adjustment, in turn, can take place by means of the long period of the spinning fiber, the degree of crystallization of the crystal, or both, as shown in Sub-Example 1.2.

Sub-example 1.5 10 Sub-example 1.5 shows the effect of a change in the tensile ratio of the mechanical drawing process of the spinning fiber, i.e. at the same time the change in the chain orientation of the fiber matrix, on the tensile strength and elongation values of the thermoset product.

15

On a conventional fiber line (Figure 1), melt-spun propylene fiber was made by mechanical drawing, using different draw ratios of fibers. The properties of the fiber polymer, the strength values of the product fibers as a function of the tensile ratio and the tensile conditions are indicated in Table 2.

(fibers D-10-14). From the obtained test fibers, test fabrics were prepared on the fabric line (Fig. 2) as a function of temperature using a conventional technique. The bonding equations for longitudinal tensile strength and elongation corresponding to the test fabrics are · 25 with their intersection points marked in Table 4.

From the equations in Table 4, it can be stated that the activation energy values corresponding to both elongation and tensile strength of the tensile process remain constant and are independent of the fiber tensile ratio within the measurement accuracy. The pre- 101087 27 exponential factor is a function of the fiber draw ratio used. In the system under consideration, the lnc values in Table 4 for tensile strength and elongation in both low and high temperature bonding regions (i.e., temperatures below and above the maximum value of 5 von) give equations: σ = T2x3,4691x1021x exp [-0,8698λ] x exp [ -48818.7 / RT] / 17 / ε = T2x6.5052x1013x exp [-1.0219λ] x exp [-33497.6 / RT] / 18 / σ = T2xl, 2090x10'7x exp [-0.4895λ] x exp [6912,3 / RT] / 19 / ε = T2x2,2027x10'14x exp [-1,0999λ] x exp [21000,6 / RT] / 20/10

The relationship between the fiber tensile ratio and the average orientation factor of the fiber polymer in the series of experiments under consideration is given as Equation / 15 / in Sub-Example 1.4. By placing this equation in equations / 17-20 /, an orientation effect is obtained on the tensile strength and elongation values of the test fabrics in the whole studied area.

In Fig. 4, the maximum tensile strength and elongation values corresponding to the equation tensile ratios in Table 4 and the course of these temperature functions have been calculated for clarity only for the tensile ratios λ = 1 and 2, respectively. Some measurement values are marked in the graphs of the functions, from which it can be stated that the equations quite well simulate the course of the measurement points.

'25 From Figure 4, it can be seen that the flow of the maximum values of the tensile strength and elongation of the test fabrics as a function of temperature is different. In the case under consideration, in the conventional operating range of thermal bonding, the tensile strength of the fiber reaches its maximum value as a function of temperature before elongation.

In order to compare the tensile strength-elongation ratios, in Table 1, in addition to the tensile strength equations, some ve-5 equation equations are indicated. The maximum tensile strength and elongation values (under the processing conditions used) of the fabric bonded from fiber B-2 are am = 65.8 N (159.4 ° C) and sm = 24.5% (153.0 ° C). Thus, at the maximum elongation temperature, the tensile strength (45.3 N) has only reached 69% of its maximum value. In the fabric made of fiber B-13, the values of maximum tensile strength and elongation are almost the same and quite close to each other in terms of temperature (42.1 N / 161.2 ° C and 42.2% / 161.0 ° C). Fabrics made of fibers B-1 and B-9 and tensile strength and elongation values are close to each other in terms of temperature, but tensile strength values are high (81.5 and 79.8 N) and elongation values are low (38.2 and 37.7%). The strength values of fabrics made of fibers A-1 and A-8 differ in both the maximum elongations and the corresponding temperatures, with the maximum value-20 hair values being quite low (Table 1.).

The elongation of the fabric (fiber) usually reacts more strongly to external influences (temperature, high energy and light radiation, etc.) than the tensile strength. These varying properties with each polymer-V 25 spinning bonding system form the basis for adjusting the strength properties of thermoset fabrics.

To demonstrate the effect of high-energy radiation, the fibers in the test series were irradiated (γ-radiation: 3.06 Mrad, stock 101087 29 ti 10 days) before bonding. The equations simulating the measured values of tensile strength and elongation of the test fabrics were of the form (T <Tm and T> Tm): σ = T2 x 1.0208x10 * x exp [-0.9427λ] expt-18766.6 / RT] / 21/5 ε = T2 X 2.9380x10 2 x exp [-0.517ΐλ] exp [-4112.9 / RT] / 22 / σ = T2 X 4.7812x10 19X exp [-0.8622λ] exp [28769.3 / RT] / 23 / Δ = T2 x 5.2692x10 19x exp [-0.7195λ] exp [28753.0 / RT] / 24 /

From Equations (21-24) and Figure 4, it can be seen that the position of both the elongation and the tensile strength of the test fabrics corresponding to the irradiated fibers have changed strongly both in terms of temperature and with respect to each other. The Akti lubrication energy values according to the equations corresponding to the tensile strength and elongation of the test fabrics are also observed to be lowered at temperatures below the shear-15 point maximum and increased at temperatures above it. It is also observed that the velocity term having a tensile ratio effect is still concentrated in the temperature-independent velocity term of the equation.

20 When bonding fibrous gauze to rollers by means of temperature and pressure, the bonding point is subjected to strong and rapid shear machining. Experimental bonding was also studied under low mechanical load in the so-called using loop binding tests.,. The link binding is performed using a thermomechanical fiber analyzer (Metier 3000). A fiber sample (50 x 2,2 dtex) is attached to each seat of the analyzer at both ends and in such a way that the resulting loops form a cross-loop with each other. This fiber loop system is loaded with a constant load of 101087 30 (1 mN / tex) and heated at a constant rate (10-50 ° C / min), simultaneously recording the elongation and temperature, to the desired "bonding temperature" and cooled. The junction of the rings formed by bonding of a strength of the mi-5 is made to tensile machine (Zwick-1435) after the both sides of the loops is cut off the other branch. The strength value (σβ, mN) of this loop bond together with the above-mentioned bonding temperature implement the conventional bonding equation / 10-12 /.

10

The strength values corresponding to the different tensile ratios of the fibers of the loop bonding test series (E: 1-5) and the molecular weight distribution of the polymer are indicated in Table 2. The equation simulating the loop bond values corresponding to the loop bond was 15 σβ = 1.0495 x 1037 x T2 x exp [-1.7219λ] exp / RT] / 25 / = 1.3684 x 1039x T2 x exp [- 8.4 954 f av] exp [- 76679 / RT] / 26 / The Akti-voiding energy values for the bonding of fibers corresponding to different tensile ratios are independent of the tensile ratios and thus correspond to the above. the binding result of conventional gauze.

The fibers of the 20 series of experiments (E: 2-4) were irradiated (γ-radiation: 3.40 Mrad, storage 70 days) and the obtained fibers were subjected to loop binding experiments. The obtained loop strengths were almost the same for the irradiated samples, i.e. the tensile ratio (orientation) effect of the bonding strength was lost (within the measurement accuracy). The equation of the loop bond strength was obtained with irradiated samples ° e.s = 7.7 7 5 2 x 1036 x T2 x exp [-76679 / RT] / 27 /

The binding result of the loop test set can be seen from Figure 5. The fiber-specific binding results (E: 1-5) have been shifted by the coefficient available from Equation / 25/101087 31 to correspond to the result of fiber E-4 taken as a reference state. The fit of the result equations to the measured values can be seen from the figure. In the loop bonding tests, the bond is subjected to a rather light mechanical load, so that the fiber to be bonded does not deform at the bonding point as in conventional thermal bonding on rollers. The partial melt formed in the loop bonding initially mainly wets the fiber bundle and as the amount of the partial melt increases, it coagulates the wetted fiber bundles to each other and finally surrounds the entire cross loop. The bonding method is not sensitive to excess melt, as this is transported outside the bonding site by the sorption effect. Changes in the fiber draw ratio are also not as sensitive in loop bonding as in roll bonding, although the mode of action of the draw ratio is similar for both. The link bonding thus mainly corresponds to hot air bonding performed with low mechanical load.

When high energy irradiated fibers were used for loop bonding, the bond strength increased in each sample of fiber. 20 regardless of the mechanical draw ratio of the fabrication, i.e., as opposed to gauze bonding. This difference can be attributed to the low fiber deformation of the loop bonding as well as to the loss of the irradiating effect damaging the polymer structure (bond chains) in the bonding process; 25 ta of the polymer part with the formation of a partial melt. The decrease in binding temperature caused by irradiation was approximately the same for both binding methods. When evaluating the loop binding experiments performed, it should be noted that small amounts of blocked amines had been doped in the polymer in addition to the basic antioxidant doping (in the gauze binding experiments) only one fiber had a low antioxidant addition). The effect of both antioxidant and some wetting additives is particularly pronounced in air binding.

The effects of thermal bonding on the values of tensile strength and elongation-10 of a fabric product obtained from fibers made with different mechanical tensile ratios and their ratios can be seen from the point of view of the control method, e.g. the following findings: A common feature of the different fiber grades and thermal bonding methods is the dependence according to equation / 14 /, where the maximum bond strength 15 (when supplied under the same manufacturing conditions) is achieved with mechanically unstretched fiber, i.e. spinning fibers. The maximum strength values of the thermal bonding can be adjusted mainly by adjusting the crystalline lamellar thickness of the spinning fiber, i.e. by adjusting the chain length and 20 distribution of the polymer, the spinning ratio of the spinning process, the cooling rate and temperature of the spinning fiber.

In industrial fabrics, it is important to provide sufficient tensile strength and elongation as well as a certain elongation / tensile strength ratio to the fabrics. The quality of the method required is determined by both the quality of the fiber used (as a function of the spinning method) and the method of thermal bonding.

101087 33

A particular problem is the control of the strength properties of thermosetting fabrics by means of a high-pressure and at the same time fast-cutting bonding equipment (e.g. roll bonding). As a result of the treatment, the fibers of the bonding point 5 are deformed, which causes fiber fractures, especially in the periphery of the bonding area. The adjustment of the thermal bonding must then be carried out on a polymer- and device-specific basis, in which case the control of the mechanical draw ratio of the fiber production and the control of the gauze bonding temperatures are essential. Adjusting the stretch-draw ratio of product fabrics always means operating below the maximum strength values of the fabrics in terms of elongation, tensile strength, or both.

The processing sensitivity 15 of thermal bonding on rollers can be reduced to some extent with skin-core fibers, especially if the melting range of the shell layer is reduced with a fiber-doped (or otherwise obtained) short chain polymer moiety (spinning distribution) or using a completely different quality.

Thermal bonding methods with light bonding machining (e.g. hot air and furnace bonding methods) avoid some of the above bonding problems. In this case, the adjustment of the binding may be simpler than with machining methods alone. However, for the large-scale production of many types of thin fabrics (from fiber gauze), these methods are poorly suited.

101087 34

Sub-example 1.6

In sub-example 1.6, the effect of the heating rate of the fiber ridge-5 gravel on the thermosetting temperatures and on the tensile strength and elongation values of the thermoset product is demonstrated by means of a series of experiments.

The thermal bonding of the fibrous gauze was assumed (Section Example 1.3) 10 to follow the general dynamic kinetic law / 10 / for the variable property of the product fabric, where the heating rate of the fibrous gauze was assumed to be constant. This is exactly how heating of the gauze in the production equipment cannot take place. In order to determine the possible deviation, a series of tests was performed, in which the transport speed of the gauze and at the same time the hot rolling speed were increased. In this case, it was assumed that the function of the heating rate of the gauze would remain the same. The speed series of the gauze web was used as the variable speed values of the binding: v, m min’1 = 35, 45, 60 and 75.

20 The properties of the test fiber and polymer used are indicated (F-1, F-2) in Table 2. The standard terms for the equations of tensile strength and elongation of product fabrics corresponding to different web speeds are indicated in Table 5.

·: 25 From the speed equations it can be seen that within the applied measurement accuracy, the binding activation energy is independent of the web speed (binding speed) in the equations corresponding to both the tensile strength and elongation of the product fabric. The magnitude of the velocity effect of the gauze web can thus be calculated from the pre-exponential factors of the binding equations. The values of tensile strength and elongation of product fabrics are given by the equations σ = V1'294 x 5.7 1 44 x 1017 x T2 x exp [-38225.8 / RT] / 28/5 ε = ν'1,223 X 6.7918 X ΙΟ17 X T2 X exp [-38225,8 / RT] / 29 /

The change in the tensile strength of the product fabrics above the temperature corresponding to the maximum value in the case under consideration (within the limits of the applied measurement accuracy) is independent of the web speed 10. However, according to the measurement results, a decrease in tensile strength is observed (after the maximum value) at high bonding temperatures (here: Ssi> 165 ° C, β <155 ° C) at each studied speed. In the case under consideration, the value of the maximum strength is about 40 (± 2) N.

15 The shear temperatures and equation parameters of the equations corresponding to this maximum strength are indicated in Table 5. The change in elongation of the product fabrics (above the temperature corresponding to the maximum value) is characterized by considerable variance. In the case under consideration, the measured values of the change in elongation 20, in the vicinity of the maximum values, can be simulated by one equation. This equation and the maximum values of elongation and temperatures corresponding to the velocities are plotted in Table 5. As the bonding temperature continues to increase, the elongation begins to decrease rapidly (too much molten phase is formed relative to the bonding requirement, machining deformation increases, oxidative aging begins, etc.). This rapid decrease in elongation appears to begin in the higher temperature range the higher the web speed. Equations corresponding to the high temperatures of elongation of the product fabrics are marked (ε2) in Table 5.101087.

The decrease in fabric elongation in the range of these maximum values (regardless of web speed) is equal to the form / 30 / se-5 and in the higher temperature ranges mentioned, as a function of the bonding speed, the form / 31 /: ε = 8.8887 x 10 "3 x T2 x exp [16888 , 3 / RT] / 30 / ε = 2.0661 x 10 "49 x v0.8774 x T2 x exp [87590.7 / RT] / 31/10

Graphs of the equations simulating the bond strength values are plotted in Figure 6. Some measurement points can also be seen in the figure.

15 For comparison, Table 5 and Figure 6 show the bond strength values (v. = 35 m min "1) corresponding to the imported fiber F-2 (Table 2.). It can be seen from the figure that the tensile strength and elongation behavior of the product fabric in bonding is similar to fiber F-2 as fiber F1, despite different values of thermal activation.

The thermo-bonding line used in the bonding speed tests tried to reconcile the main speed differences between the karst rolls and between them and the bonding rolls so that the final | The deflection values would be constant at different web speeds in the test series. The constancy of the tampon values was monitored by analyzing the ratio of the longitudinal and transverse tensile strength of the test fabrics. According to the calculations, only a maximum deviation of 4.7% was observed at the highest web speed.

The adjustment of the strength properties of product fabrics in thermal bonding 5 is based on e.g. to the following experimental observations - both by adjusting the web speed and the setting temperature, the strength values of the fabrics can be adjusted within wide limits, especially when operating below the maximum values of the strength values and their corresponding temperatures. The results 10 also show a high effect of polymer-doped antioxidant blends on both tensile strength and especially elongation values at temperatures above the maximum strength values - it is also important for both production and control that the higher the bonding rate, the lower the bonding rate. delay.

Sub-Example 1.7 20

Sub-Example 1.7 considers the effect of fiber cable tension in the melt spinning process on the thermal bonding of the resulting product fibers.

• The chain orientation that develops in melt spinning is mainly controlled by the melt flow rate field and, in contrast, the structural relaxation caused by the thermal motion of the molecules. Due to the low velocity gradient and the short relaxation times caused by the high nozzle temperature, the orientation in the region of the capillary flow (in the nozzles) is low in stability and insignificant. The kinetically stable chain orientation of the fibers occurs only during the melt stretching flow, where the orientation-controlling fiber axis flow rate is high and the melt viscosity increases with decreasing temperature increases the molecular relaxation time (preventing disorientation) and finally the melting solidification. It can be shown that the stress acting on the fiber filament at the pour point and the birefringence of the fiber polymer are both in proportion to the melt spinning ratio, and thus the tensile strength of the birefringence and the pour point are also directly proportional to each other. The tensile stress at the solidification point, in turn, is approximately the same as the tensile stress at the l-galet (Figure 1.). Thus, factors affecting the increase in spinning tension also increase the chain orientation of the fibrous filament. The increase in spinning tension is promoted by e.g. factors: increase in polymer viscosity, decrease in spinning temperature, increase in spinning capacity (at constant titer), decrease in fiber titer, increase in quench rate, etc.

25 Using some examples, let us consider the effect of the tension of a fiber cable in a melt spinning process on the thermal bonding of a fiber. Table 6 shows the standard terms for the bonding equations for the strength values of the fabrics responsible for the thermal bonding result of the fiber sets under consideration, the fiber cable stresses corresponding to the bonding equations (SLT: N / spinning cable number 30500-), and the crystallinity degrees of the polymers. The spinning ratio of the test fibers was = 206 and the mechanical drawing ratio, λ = 1.15 5 (for samples H-7 and H-8: λ * = 189, λ = 1.25), and the titer of the staple fiber was 2.2 dtex. The weight of the product fabrics was on average, w = 23 g / m2. The tensile strength-elongation curves of the test fabrics corresponding to the bonding equations are indicated in Figure 7.

10 Figure 7 shows the results of thermal bonding corresponding to the test fibers H-1 and H-2 (SLT: 41 and 57N) as values of the tensile strength-elongation functions of the fabrics with bonding temperatures and cable stresses as parameters. According to the figure, the bonding equations, respectively, are found to pass through the maximum of the strength values of the fabrics as a function of temperature. It is further seen that as the SLT value decreases, the strength values increase for all isotherms before the maximum values and decrease thereafter. Before reaching the maximum values, the changes in the strength values as a function of the SLT values are quite noticeable, but low after the isotherms.

Fiber samples H-3 and H-4 are made of a polymer having the same melt index but a chain distribution • - 25 substantially narrower than the polymer corresponding to samples H-1 and H-2. It can be seen from Table 7 that the fabrics obtained from the test fibers (H-3 and H-4) have low strength over the entire binding area compared to the test series discussed above. From the graphs of the bonding equations 101087 40, it can be seen that the effect of SLT is low with respect to the elongation values below the elongation maxima, but considerable with the isotherms above them. By adding a more effective antioxidant mixture to the polymer in question, the effect of SLT can be completely eliminated from the stretching isotherms over the entire bonding temperature range [Fibers H-31 and H-41, SLT: 24 and 41N: high / temperatures: E (σ) = 34684, 4, In c = -48.7365, am = 39.2 N / 433.7 ° K; E (ε) = 34684.4, In c = -49.1619, mp = 31.4% / 431.4 ° K / H-31 10 and In c = -49.2113, mp = 30.0% / 431.4 ° K / H-41].

In the thermal bonding of fiber samples H-3 (-31) and H-4 (-41), control methods based on both the bonding temperature and the spinning cable tension play a rather small role.

15 A third consideration is the melt spinning of a polymer with a melt index of 25 and a wide chain distribution. The standard terms for the equations corresponding to the thermal bonding results of fibers H-5, H-6 and H-7, H-8 prepared with mechanical tensile ratios, λ = 1,15 and 1,25, are given in Table 6. The tensile strengths of the test fabrics corresponding to fibers H-20 5 and H-6 the elongation curves are plotted in Figure 7.

It can be seen from the figure that the effect of the tension of the spinning cable is quite low with respect to the tensile strength of the fabrics at different isotherms. With respect to the elongations of the fabrics, the effect of SLT-25 is significant only at the temperatures following the elongation maxima, where the elongation values decrease isothermally as the SLT value decreases.

From the bonding equations corresponding to the test fibers H-7 and H-8 (λ = 1.25), it can be seen that the SLT values affect the thermal bonding result over the entire temperature range. Before the maximum of the strength values, a decrease in the SLT value increases the tensile strength and elongation values of the fabrics, and after the maximum, it increases the tensile strength and decreases the elongation values.

5 Finally, consider melt spinning with a fiber polymer having a melt index of MI = 18 and chain distribution values, MWD: 221000-6.4. The polymer chain dispersion is thus the largest of those studied. Under the quenching conditions corresponding to the test series considered, this polymer also gives the highest values of melt-spinning cable stresses in the series 10.

According to both the equation constants in Table 6 and the function curves in Figure 7, as the tension of the spinning cable decreases, both the tensile strength and tensile values increase with each isotherm over the entire temperature range. However, the strength changes are greatest for the 15 isotherms before the maximum strength values.

At the beginning of the sub-example, some factors affecting the spinning stress are listed. In the production of high-strength, high-orientation monofilaments, spinning stresses play an important role in the formation of fiber orientation. In the production of fibers with a relatively low orientation, the effect of easily implemented spinning tension changes is low. In this case, the mo- ». ·; 25 in the analysis of the thermal bonding strength of nifunctional fibers, the effects of spinning-stress variations in the manufacture of fibers, often difficult to distinguish from a number of other factors. However, in the control of the strength values of thermosetting, the control of the spinning stresses 101087 42 plays an important role, especially in the manufacture of disposable fabrics when adjusting their required low limit strengths.

5 10 15 20 25 101087 43

Example 2.

Example 2 briefly examines some of the determinants of thermal bonding of skin-core structured fibers.

5 The sub-example examines the behavior of 'nested layer fibers' containing either two different grades or two polymers of the same quality and one polymer of the same quality but modified after spinning.

10

Sub-example 2.1

Sub-Example 2.1 considers bicomponent fibers made from two different grades (limited to 15 ti soluble) of polymers using nested nozzles in spinning. The skin pairs of the heat-bondable fibers obtained form the polymer pairs: polyethylene / polypropylene (PE / PP fibers 1-1 and -2, Table 2.), polyethylene / polyethylene terephthalate (PE / PET fiber 1-3) and. 20 polypropylene / polyethylene terephthalate (PP / PET fiber 1-4).

The values of the standard terms of the bonding equation / 12 / corresponding to the strength values (σ and ε) of the fabrics obtained by thermally bonding polyethylene / polypropylene test fibers 1-1 and -2 are given in Table 7. The graphs of the equations and some values of the measurement points are shown in Figure 8. the measurement results corresponding to both test fibers are consistent with the measurement accuracy used. There is a transition range between the measured values corresponding to the low and high temperature ranges according to the equations, where the measured values do not implement either equation. It should also be noted that the activation energy terms of the bonding equations corresponding to the tensile strength of both measurement regions are of the same sign, so that in both regions there is an increase in tensile strength as the temperature increases.

To clarify the function of the binding sites on the bicomponent test fibers, a series of TMA-10 loop experiments were performed on these fibers (Sub-Example 1.5). The standard terms of the bonding equations corresponding to the loop experiments are indicated in Table 8. DSC analyzes of the test fibers are also indicated in the same table, from which the melting and solidification points (enthalpy peaks) and crystallinity degrees of the polymers can be determined.

To understand the behavior of the melt phase promoting thermosetting, the temperature distributions of the cross-sectional area 20 (in the normal direction of the fabric surface) of the bonding site of the pure polypropylene fiber fabric as a function of the velocity of the fiber gauze have been calculated. The calculation uses the known Bin-der-Smith difference method and the Gröberi distribution function for the initial values. In performing the calculation, it is assumed that for each gait rate determined by the five- «·; The 25 faults have the amount of heat required for the binding transferred to the binding. The temperature difference between the binding rollers, Δθ = 15 ° C, has been taken into account in the calculation. The strong anomaly of heat transfer rates and specific heat in the audited area ai 101087 45 casts the qualitative value of the calculated values, but the necessary essential information is obtained from the distribution.

According to Figure 9, the temperature profiles of the bonding point are mainly similar in shape to the parabola. As the bonding rate increases, the temperature decreases rapidly in the interior of the bond near room temperature and increases significantly in the surface portions and surface of the bond (by the amount of heat given to achieve thermal equilibrium). The temperature difference of the roll surfaces in the system does not seem to have a large effect on the position of the temperature-10 minimum in the cross section. From the calculated temperature profile, it is obvious that the temperature inside the cross-section of the bonding region does not rise so high at the technical bonding rates that the partial melting of the polymer (PP) would produce the amount of melt required for bonding. The surface parts of the bond at a sufficiently high temperature must thus produce a molten polymer (either wholly or partially melted fibers) which, as a result of the compressive and shear machining of the bonding rolls, shifts to the inside of the bond stack to cause cold and heat bonding. This conventional "thermobonding mechanism" with one-component fibers is also applicable to the two-component fibers under consideration.

The TMA results of the loop tests of the PE / PP fiber system can be ·; It can be observed that the elongation values of the system reach a minimum in the temperature range, 9 = 90 ° -100 ° C. The conventional thermal shrinkage curve following the elongation minima (9 = 95 ° -161 ° C) has an anomalous temperature range between 9 = 118 ° -125 ° C). The application begins as a shrinkage inflection point at 10 = 118.7 ° C, continues to a shrinkage peak at θ = 122 ° C, and ends with a small elongation minimum at θ = 125 ° C. This area is caused by the melting of the shell layer of the fiber system.

5 In the loop experiments, the bonding of the fibers starts at a temperature, θ = about 112 ° C, and the bond strength increases according to the partial melting of the polyethylene layer according to the bonding equation 1-1 (Table 7, I-1: 3). After the melting range of ethylene, the increase in bond strength is divided into two ranges as a function of temperature, both in terms of strength values and activation energy (Table 7, 1-1: 1 and 2). The strengths of the loop bonds can be approximated by the equations (θ = 127 ° -160 ° C): σ1 = 18.18 θ - 1581.6 / 32 / and σ2 = 21.95 θ - 2443.7 / 33/15 In sub-example 1.5 it was found that the loop bond corresponds to mainly hot air and furnace bonding, which differs from roll bonding mainly in the absence of compression and shear machining. In the loop bonding of the 2-component fibers under consideration, the transition regions of tensile strength and elongation corresponding to the fabric tests do not exist as such. After the melting of the polyethylene phase, as the temperature rises, the strengthening of the loop bonds (E-values negative) takes place in a manner corresponding to the fabric bond. Thus, the areas immediately following melting could be considered as transition areas where the strength values of the loops fluctuate and the elongations are low. The observed scattering of strength values in this range would result from both the increase in PP solubility in the PE phase caused by the long melt lag time of the loop experiments and the solidification of 101087 47 PE + PP melt phase as separate or same crystallization as separate or same crystallization (separate crystallization in the range in the range 136-140 ° C, co-crystallization: PE + PP solidifies in the range 115-119 ° C). A similar phenomenon 5 did not occur in the thermal bonding of some production fiber batches. It should also be noted that a strong increase in the amount of melt (mutually soluble PE + PP particle melt) may not be advantageous for thermosetting. In the loop tests the excess melt can flow above and below the fiber bundle binding site.

10 The TMA results of the high-temperature range of the link bonding experiments show the partial melting of polypropylene and the related large increase in the thermal shrinkage of the system and at the same time the link bond strength.

The gauze bonding tests corresponding to the test fibers 1: 1 to 6 have been performed using a temperature difference, Δ3 = 7 ° C, between the smooth and embossed roll. When investigating the significance of the magnitude of this gradient in thermal bonding, it was found that by decreasing the temperature gradient by raising the temperature of the patterned roll, both the tensile strengths and elongations of the test fabrics increased strongly. This is a significant finding, especially with respect to fabric elongations, as these usually decrease with increasing temperature. According to the measurement results, the following equations (T = Tsi) are obtained as equations (T = Tsi) describing the effect of the gradient A (= δsi-Spi) on the 1-1 and -2 thermosets of test fibers: σ = 8.8289 x 107 x T2 x exp 1018 x ΙΟ'2 x Δ] x exp [-23054,5 / RT] / 34/101087 48 ε = 1.7087 χ ΙΟ'5 χ Τ2 χ exp [-3.6862 χ ΙΟ'2 χ Δ] χ exp [+ 1720.7 / RT] / 35 /

The effect of gauze web speed on the thermal bonding of PE / PP two-component fiber was investigated in 5 scale runs on a production scale. The increase of the web speed between v = 36-60 m / min weakened both the tensile strength and (slightly) also the elongation values of the fabric in all conditions.

In this connection, it can also be stated that the structural factors influencing the temperature, solidification and thermal bond strength values of the polymer 10 are, in addition to the quenching temperature and rate and the degree of crystallinity, the values of the chain length and distribution of the polymer. In particular, the high value of the chain distribution is one of the prerequisites for the good strength properties of fabrics. In the case of bicomponent fibers, this applies in particular to the polyethylene of the shell layer, which has a low dispersion value of ordinary grades. Examples include some polyethylene chain size values (Mw / D): 33110 / 2.56, 42650 / 2.94, 55500 / 3.35, 2048960 / 4.36, 56000 / 5.17, etc.

Binding roller temperatures ($ si) have been used to examine the thermal bonding of fiber gauze. In Table 7, the equation constants for the fiber binding equation I: 1-2 have been calculated so that • 15 ° C, i.e. T =, was subtracted from the temperatures of 25 smooth rolls.

Tsi-15 to approximate the actual temperature in the bond. It can be seen from the table that the effect of the temperature change on the activation energy values is quite significant. Thus, the differences in the activation energy values of the loop and gauze bonding cannot be explained by the temperature differences of the systems.

Table 7 shows the constants of the equations corresponding to the bonding test series of some PE / PP two-component-5 fiber batches (I: 6-14). It can be seen from the table that the activation energy values of the bonding equations corresponding to the fiber batches differ considerably, especially in the region of low temperatures. These differences are already due to the differences in the amount and solidification of the melt and the presence of different types of surfactants (finishes, antioxidants, etc.).

The two-component fibers, in which the fiber core is polyethylene terephthalate and the fiber shell is either polyethylene or polypropylene, behave according to the TMA results with respect to thermos-Donna analogously to the fiber systems discussed above. However, the polyester fiber did not participate in the bonding process in the temperature range studied. The melt bonding of the PE and PP phases of the polyethylene and polypropylene coated fibers (I: 3-5) is followed by a decrease in bond strength as the temperature increases due to both aging and other causes (Table 8). In fiber gauze bonding experiments corresponding to both fiber grades, the bonding of the shell layer in its melting range corresponds to the PE / PP fiber system (e.g. 1-3 and 1-6). However, unlike loop tests, PE / PET fibers still have a slight increase in the tensile strength and elongation values of the fabrics after the melt bonding of the shell layer, which may be due to the difference in different processing times (aging and other phenomena). It should also be noted that the reduction of the temperature difference of the bonding rollers did not significantly affect (unlike the PE / PP system) the strength values of the fabrics in either PET core fiber.

Sub-example 2.2

Sub-Example 2.2 considers the thermal bonding of two skin-core fiber sets made of polypropylene in different ways.

In the first set of fibers (Table 2, D: 7-12), the skin-core structure is obtained as a result of peripheral oxidation of the superheated spinning fiber and concomitant slow quenching caused by polymer chain degradation. A layer of low-melting, short-chain polymer is then formed on the fibrous surface, which is coherent with the long-chain core polymer. The product fiber has a high degree of crystallinity. Peripherally oxidised bed fibers

• The 20 dun manufacturing method is described e.g. U.S. Pat

5.281.378 / 1994 in the specification and prior art.

In the second set of fibers (Table 2, B: 1,4,6,8,12), the skin-core structure is obtained in a simultaneous rapid spinning process of a very short-chain and long-chain polymer. The product fiber is then low in monoclinic crystallinity and 'super-crystalline' in structure.

101087 51

The values of the standard terms of the bonding equations corresponding to the tensile strength of the fibers produced by the peripheral oxidation method are plotted in Table 9, from which the DSC analysis results of the corresponding fibers can also be seen.

5 Briefly, the results of the oxidation test series performed on the spinning and thermos-Donna of the fibers are as follows: - The D121 sample of Table 9 was spun at a temperature of 3 = 292 ° C, spinning ratio, Xk = 210 and mouth-10 spin speed, v = 0.389 m / min, without slowing down the cooling rate. Spinning of sample D10 was performed at the same melt temperature as sample D121, but quenching of the sample was slowed by reducing the nozzle speed to v = 0.25 m / min and reducing the amount of quenching air (21 ° C) by about 15 50% of the initial value (V = 735 m3 / h with capacity, P = 31.8 kg / h, d = 2.2 dtex, λ = 1.15), whereby the spinning ratio has increased to λk = 1630.

It can be seen from Table 9 that due to the changes, the value of the activation energy (E, kcal / mol) of the bonding equation corresponding to the tensile strength of the fabric has decreased from | e | = 48.7 to | e | = 20.8. Correspondingly, the maximum values of tensile strength and elongation values have changed in the range of values, σ: 39.5-56.5 N and ε: 72-89%. In particular, a decrease in the temperature corresponding to the tensile strength maxima due to the slowed quenching is in the range of 3 = 157.9 ° -153.0 ° C.

Delayed quenching and reduced nozzle speed have been used in the preparation of fiber sample D12, but at the same time the spinning melt temperature has been reduced by 7 ° C. The maximum values of the tensile strength and elongation of the bonding equation decreased 101087 52 then substantially, i.e. to the values, σ = 27.7 N and ε = 34.0%. Sample D12 is not directly comparable to Sample D10 because their manufacturing draw ratio values differed.

5 - In the fiber samples D: 7-11 of Table 9, the spinning conditions in the furnace are similar in terms of each other, but the quenching of the fiber melt is slowed down mainly by reducing the quench gas volume (pressure, p = 300-50 Pa, cable tension, SLT = 18-11 N) . Some samples also have a reduced mechanical draw ratio of 10. According to the table, the maximum values of the draw ratios and elongations of the bonding equations change only slightly as the amount of extinguishing gas decreases. However, the temperatures corresponding to the maximum values decrease considerably. As a result of chain breakage following peripheral oxidation, the melt indices (MI, ASTM D1238) of fiber samples increase rapidly as a function of oxidation. Between the activation energies of the bonding equations and the melt index ratio of the corresponding fiber samples, SMI (melt index of the fiber / melt index of the original polymer), the equation E = -77906 + 15519 x SMI / 36 / is obtained within the applied measurement accuracy.

A similar equation can also be obtained between the melt index ratio and the bonding temperatures corresponding to the maxima of the strength values of the bonding equations.

25 - The relationship between the maximum values of the tensile strengths of the fabrics and the crystalline lamellar thickness found in Section 1.4 is realized and can be demonstrated in cases where it is determined by SAXS analysis (in most cases by combined SAXS and Ra-101087 53 man spectrum analysis). The relationship between the mechanical tensile ratio and the maximum values of tensile strength also seems to be realized.

5 Let us briefly consider the behavior of skin-core structured fibers made of polypropylene by means of spinning and quenching processes in the thermal bonding of fiber gauze and loop. WAXS analysis of test fibers usually shows smectic structure and thus very low monoclinic crystallinity. SAXS analysis, on the other hand, shows a structural anomaly. The first-order SAXS peak is difficult to obtain from the measured intensity and angular values. Lorenz-corrected intensity values usually give a strong peak in addition to the first 15-order peak, which is mainly zero-angle scattering. The SAXS anomaly is caused by the different lamellar structure systems of the shell and core layers of the fiber, from which the scattering sum is obtained by analysis.

20 The properties of some of the fibers in this group and the standard terms of the bonding equations are given (B: 1,2,4,6,8,12) in Tables 2 and 10.

Test fibers were made from the same polymer grade (Mw = 225.2000, Mn = 37600, D = 5.93). The strength values of the test fibers approximate the equation σ = 771.7 x ε’0.6117, (omN / dtex; ε%). The tensile strength-elongation ratios of the fibers are characterized by a clear yield point. The test fibers comply with the dependences between fabric strength and fiber structure indicated by sub-pre-101087 54 mark 1.4, i.e. amax = F (D (Z}, λ, fav).

From the results of the thermomechanical loop tests of the fiber series B under consideration, it can be seen that the elongation maxima of different fiber grades differ in both position and size. There is also obvious dispersion in the fiber-specific elongation results due to the nature of the loop bond (low initial load: lmN / tex). The position of the thermomechanical shrinkage with respect to temperature is the same for different fiber samples (of the same fiber grade) and no dispersion occurs. The central bonding of the loop fibers always begins at the temperatures of the base portion 15 of the TM shrinkage peak and generally reaches its maximum strength at the temperatures of the TM peak. As the temperature rises above the temperature corresponding to the TM shrinkage peak, the bond strength decreases immediately.

According to Table 10, the values of the activation energy of loop and gauze bonding of fiber grades B-4, -6 and -8 (Table L and Y) are close to each other on a fiber-by-fiber basis. For the bonding comparison, the bonding heat-25 states corresponding to the loop equations of 100 mN and 1000 mN have been calculated from the bonding equations. These strength values are close to both beginning and ending reinforcement. According to Table 10, the bonding with said fibers starts at a temperature of 131.4 ± 0.4 ° C and reaches a limit of 1000 mN depending on the activation energy values in the temperature range of 148-151 ° C. In fabric bonding, the link strengths of the fiber grade B-1 having the best bond strength are set higher at the above-mentioned link strengths (Δθ = 143.1-159.4 ° C). At very high temperatures and low strength, the gauze-binding fiber grade A-1 5 (Tables 1 and 2, loop: E = -38766, In c = 40.1979, Δβ = 136.6-156.5 ° C) settles at lower temperatures than the fiber grade B-1 in loop bonding. The advantageous location of the fiber grade A-1 in the loop bonding is mainly due to the fact that in this bonding method, for example, the fiber surface finishing agent vii-10 does not interfere with the strengthening of the bond corresponding to the machining bond.

Fiber grade B-12 is set in loop bonding exactly to the values of fiber grade B-1. With this fiber grade, which is already close to a conventional homogeneous polypropylene fiber, a high temperature 'aging zone' is also observed.

For a key comparison of fiber set B and the fiber sets already considered, some values of the number-20 binding equations of the sets and their derivatives are given in Table 11. The binding equation corresponding to fiber designation A-15 is the average of the binding equations of fifteen A-series fiber batches. Fiber C-2 is a bicomponent fiber in which both the core and the shell layer are propylene polymers with different melting ranges. The table shows the derivative of the tensile strength of the bonding equation with respect to temperature at (θ30 ° C), where the bond strength corresponds to the minimum value required of the fabric (in this context), σ = 30 N.

The fraction corresponding to the minimum strength of the maximum strength 101087 56 (a) is also indicated in the table, as is the derivative da / dT, with the fraction corresponding to the minimum strength.

It can be seen from Table 11 that the temperatures corresponding to the maximum strength values are close to each other e.g. in fiber series B and in the average series A-15.

However, at the minimum level of fabric strength requirements (σ = 30N), the bond strength is only 37% of the maximum value in the B-1 series and already 78% (100a) in the A-15 series, with deri-10 garments at da / dT close to each other. Although the temperatures corresponding to the maximum bond strength of the test series are close to each other, the bond strength corresponding to the minimum level is achieved in the B-1 series at 11.9 ° C lower than in the A-15-15 series. Only at high temperatures does the A-1 fiber quality, which binds and has low strength properties, reach the minimum strength only at a temperature 18 ° C higher than the B-1 series.

The fiber grade B-2 in the table shows the effect of the unusually low activation energy of the bond on the θ30 temperature. In the fiber samples of fiber set D, a decrease in $ m temperatures occurs, with the om values remaining approximately equal. In the D-series fibers, as the thickness of the shell layer formed by the short-chain polymer increases, the activation energy values decrease and, consequently, the ilan30 temperature decreases relative to the Sm temperature.

101087 57

The most important findings of the method description related to the control method are listed below:

Most of the variables and parameters affecting the thermal bond strength strongly correlate with the bond temperature, which has been taken as the main variable of the control method both for this and for some kinetic reasons. According to the measurement results, the thermal bonding can be considered as a thermally activated process which follows the Arrhenius-type heat-shrinkage due to the narrowness of the functional heat-10 space range.

In the dynamic control equation simulating the measurement results, instead of the value of the linear heating rate of the bond 15, the value of the speed of the gauze web is assumed and a simple dependence between these speed values is assumed. According to the measurements, this dependence can be described in the area under consideration in addition to the constant factor, with a velocity exponent close to one.

20

As a result of the mechanical tension of the fiber following spinning, the bond strength of the fiber gauze decreases exponentially as the tensile ratio increases, which at the same time shows the best strength properties of nonwoven fabrics obtained with spinning fiber.

• The 4 '1 25 draw ratio effect does not, of course, reduce the bond strength values when bonding, for example, fixed skin-core multicomponent fibers in which the bonding occurs by a shell layer phase with a lower melting temperature range than the core layer phase and a temperature range above this melting point.

The increase in strength properties as a function of temperature 5 according to the control equation is followed by a decrease in strength values at high temperatures due to thermal aging of the polymer, autogenous oxidation, mechanical deformation, increase in melt volume and other factors. In order to monitor the strength properties of the thermal bonding of this temperature range, the control method (for analogous reasons, etc.) uses a control equation of the same form as even at low temperatures.

The point of intersection of these control equations is used in the so-called method. as the maximum control strength, the value of which is usually close to the maximum values of the measured strengths (and the corresponding temperatures).

According to the experimental measurement results, the control strength values of the nonwoven fabrics and the corresponding temperatures are functions of the inverse value of the crystalline lamella thickness of the spun fiber polymer structure 20. According to measurements (TMA, DMS), thermobonding begins in the temperature range where the thermomechanical shrinkage of the fibers and the disorientation of the molecular chains begin. This temperature, including the onset of partial melting of the polymer structure, is a function of the inverse of the crystalline lamellar thickness of the polymer structure.

The crystalline lamellar thickness of the polymer structure is thus a rather important control variable related to the control method.

101087 59 The crystalline lamellar thickness of the polymer structure used in the control method is reported as the product of the Lorenz-corrected long identity period and crystallinity degree fraction of the polymer. Both input factors are determined directly from fiber 5 by X-ray diffraction analysis (SAXS and WAXS).

From the SAXS measurement results performed for the control method, an equation was constructed to determine the long identity period. In the temperature range of thermal bonding, sufficiently accurate period values are obtained from the equation as a function of temperature and time for control estimation.

To determine the increase in crystallinity as a function of time and temperature, measurements were performed on some fiber polymers. From the measurement results, it was found that the Avrami-type kinetic equation is suitable for monitoring the degree of hardness of secondary crystallization. However, fiber polymers have very little in common in their crystallization ratios, so when using different quality fiber polymers, the kinetics of post-spinning crystallization must always be determined.

* 20 The crystalline lamellar thickness of a fiber polymer is adjusted by adjusting its long period and crystallinity values both in the production of spinning fiber and, if necessary, by annealing the fibers during processing under the control of the mentioned period and crystallinity equations. In the control method, if the control accuracy remains good, the period values of said period equation and the spinning fiber can be used in parallel, despite their different generations (as well as a slight difference in size from the control point of view).

101087 60

The long identity period of the polymer structure of the spinning fiber is almost exclusively a function of the degree of subcooling of the polymer melt and can be adjusted (especially with respect to the minimum value) by the conventional quenching temperature control of the spinning fiber.

The degree of crystallinity of the spinning fiber polymer is controlled by the melt quench rate. The temperature corresponding to the quench rate of the spinning melt, which is relevant to the future polymer structure, has been found to correspond to the temperature of the maximum value of the crystallization rates of the polymer. As an almost linear function of the logarithm of the quench rate corresponding to this temperature, the desired spinning fiber structures and degrees of crystallinity are obtained.

The values of the activation energy of the thermal bonding control equation depend on the fiber structure and its error states, the bonding method (e.g. the applied bonding pressure), the melt formation and amount, and several other factors. For this reason, the value of the activation energy of the bonding corresponding to each fiber grade needs to be determined either by pilot or TM loop measurements or also by the temperature dependence of the unloaded thermal shrinkage of the fiber. Below the maximum values corresponding to the strength properties of the thermal bond, the values of the activation energy of the longitudinal and transverse tensile strength are equal to each other. The same is true for product extensions. The activation energy values corresponding to the tensile strength and elongation values of the product fabrics may differ much depending on the fiber quality (e.g. fibers with a plastic component and skin-core structure). In the temperature range exceeding the maximum values corresponding to the strength properties, the activation energy values are usually below the values corresponding to the low temperatures and sensitive to pressure fluctuations and melt volumes.

In estimating thermal bond strength values and control equation for parameter measurements or product design, the value of activation energy, E = 40 ± 3 kcal / mol, can be used in the low temperature range, especially when 10 maximum strength values and corresponding temperatures are determined by the crystalline lamellar thickness of the fibrous structure. For the high temperature range, the values of polymer grade viscose flow can be used in the estimation as well as the general dependence function can be utilized, according to which the pre-15 exponential factor is the same linear function of the activation energy in both temperature ranges.

When measuring the strength properties of thermal bonding, it was found that the line pressure between the bonding rollers has a rather low effect on the bond strength values after exceeding a certain ‘critical’ pressure limit. In the measurements performed, this pressure limit was 50 ± 5 N / mm. In most of the test runs performed in this study, the line value-25 near value, 60 N / mm, has been considered a permanent parameter. When operating above the temperature corresponding to the maximum of the strength properties, and especially when the amount of polymer melt is large (skin-core structured and other fibers), the bonding pressure corresponding to the optimum result must be adjusted (below the limit value).

In the method of adjusting the strength values of thermal bonding, the cable tension (SLT) of the spinning fiber fabrication and the temperature difference of the bonding rollers, both of which affect the values of tensile strength and elongation of the nonwoven fabric, have been considered as 5 parametric variables. As parametric variables, these are included in the pre-exponential term (c) of the temperature function of the control equation.

The cable tension of the spinning fiber is a function of the molecular size and size distribution of the polymer chains and the cooling technique of the spinning melt. The cable tension affects e.g. through the orientation of the molecular chains of the crude polymer and the lamellar crystal thickness formed in the crown-15 to the strength of the spinning fiber. Depending on the spinning system used, the SLT effect can be quite significant in adjusting and standardizing the strength properties of fabrics. Due to the multi-functionality, the SLT values applied in spinning must be kept in the process, preferably on a fiber-by-fiber basis, preferably parametric, but subject to continuous, precise control.

The temperature difference between the gauze bonding rollers required for processing is polyfunctional and is determined by the velocity and basis weight (i.e., thermal load) of the gauze web, melt rates required, asymmetric temperature profile of the bonding cross-section, Only one example of the use of this complicated temperature difference effect in adjusting the strength properties of fabrics is given in the method description. However, the optimization of the required temperature difference must always be performed on a fiber-by-fiber basis and for this reason it is used in the method under consideration as a parameter in the overall control of the production process.

In connection with this review, the method of adjusting the strength properties of thermosetting fabrics has been applied mainly to gauze bonding by means of bonding rollers. However, in addition to roller bonding, air-furnace bonding has been performed with directly correlated thermomechanical test runs as well as vertical measurements using different bonding methods using gamma-irradiated fibers.

In cases corresponding to air and furnace bonding, the bond strengths follow the usual exponential dependence of the mechanical draw ratio (or the average molecular chain orientation of the fiber structure) in roll bonding and decrease sharply as the draw ratio (chain orientation) increases.

However, this draw ratio effect does not apply to skin-core structured fibers in which the shell layer polymer has a melting temperature range well below the core fiber polymer and a high amount of melt phase at the bonding temperature (e.g., polyethylene-polypropylene nested fiber). In this case, the thermal bonding corresponds to the bonding above the maximum temperature corresponding to the strength values. If necessary, these fibers can be drawn to a high degree of chain orientation already in the spinning process or also mechanically after spinning. The bonding strengths of the irradiated fibers lose said exponential draw ratio effect and the bonding strengths correspond to the strengths of the spinning fiber, i.e. the bonding strengths of the air and oven bonding 5 were substantially improved by the irradiation of the fibers. In addition to the improvement in bond strength, the bond temperatures also decreased, with the amount of decrease being a power function of the fiber draw ratio. In roll bonding, the strength properties of the irradiated fibers decreased substantially, but the bonding temperatures preferably decreased as a function of nearly the same draw ratio as in air bonding.

The control of the strength properties of the thermosetting nonwoven fabric 15 is controlled by a control equation with the main variables being the bonding temperature, the speed of the gauze web and the mechanical tensile ratio of the fibers to be bonded. Variable parameters that are less frequently subject to change in production processing, but by no means less important, are in particular the crystalline lamellar thickness of the spinning fiber structure, the tension of the spinning cable, the temperature difference of the bonding rolls and especially the maximum strength values above the casting temperature.

; If desired, the variable parameters can of course be placed in the control equation in a manner corresponding to the speed of the gauze web and the draw ratio of the fiber, and thus it is advantageous to perform, for example, product design under control equation 101087 65 in pilot or production experiments to match desired fabric properties.

In this context, it should be noted that in the manufacture and use of prior art homogeneous or layered fibers 5 per se or in fiber blends for thermosetting nonwoven fabrics, the required strength properties and ratios are met by the control method in which case different cost factors also determine the processes to be chosen and the technology to be applied.

The method description shows the implementation of a new control method for both fiber and fabric. It should be noted that the highly complicated method of controlling the manufacturing processes of the fibers and nonwoven fabrics made therefrom according to the invention can be varied in a wide variety of ways while still remaining within the scope indicated by the examples and claims.

Attempts have been made to theorize the phenomena related to the control method in connection with the examples in order to give a clear scientific picture of the method according to the new invention. However, it is self-evident that not all • phenomena related to the method have been explained, either in the absence of their unknown nature or in the absence of adequate technical and scientific measurement results, so the criteria given in the description of the new method cannot be relied on alone.

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Referenced by: / 1 / A. Watzl:

Melliand Textilberichte, 10, 1994, 840-850; 11, 1994, 933-940; 12, 1994, 1015-1020; 1-2, 1995, 76-78; 3, 1995, 170-173; 4, 1995, 265-269 / 2 / S.B. Warner:

Textile Res. J., 1989, 151-159 / 3 / D. Miiller:

Chemiefasern / Textil, 37, 1987, 704-708 Nonwoven Report International, 24, 1988, 28-31 INDA JNR, 1, 1989, 35-43 INDA JNR, 6, 1994, 47-51 (D. Miiller, S. Klöcker ) / 4 / S. Klöcker - Stelter:

Dissertation, Bremität Universenät, 1992 "Entwicklung eines Processmodelles zum Verhalten textiler Gebilde im Spalt biegekompensierter Walzenkalender am Beispiel der Vliesverfestigung" / 5 / F.T. Gilmore, R. Dharmadhikary: INDA JNR, 5, 1993, 38-42 T.F. Gilmore, Z.X. Mi, S.K. Satra: TAPPI Proceedings, Nonwovens Conference 1993, 87-92 T.F. Gilmore, R.K. Nayak, M. Mohammed: INDA TEC '92 Proceedings', Ft. Lauerdale, FL,

April 7-10, 1992, 249-259 / 6 / T.F. Gilmore, N. Timble: INDA JNR, 6, 1994, 30-37 / 7 / S. Misra, J.E. Spruiell, G.C. Richeson: INDA JNR, 5, 1993, 13-19! ’/ 8 / A.C. Smith, W.W. Roberts, Jr .: INDA JNR, 6, 1994, 31-40 ΙΟΊ 08/82/9 / Κ.γ. Wei, T.L. Vigo: J. Appl. Polym. Sci., Vol. 30, 1985, 1523-1534 J.C. Shimalla, J.C. Whitwell:

Textile Res. J., 1976, 405-417 P.E. Gibson, R.L. McGill: TAPPI Journal, 1987, 82-86

Wo K Kwok, J.P. Crane, A. A-M. Gorrafa, Y. Iyengar:

Nonwovens Industry, 1988, 30-33 C.K. Deakyne, L. Rebenfeld, J.C. Whitwell:

Textile Res. J., 1977, 491-493 A. Drelich:

Nonwovens Industry, Sept. 1985 EDANA Index 90 Congress, April 3-6, 1990, Geneva, Switzerland:

Technology 1.

/ 10 / R.J. Kerekes:

Trans. Tech. Section (Can. Pulp & Paper Assoc.), 5, 1979, 66-76 / 11 / G.A. Kinney: US 3,338,992 / 1967, US 3,341,394 / 1967 M.R. Record: US 3,276,944 / 1966 J.C. Petersen: US 3,502,538 / 1970 L. Hartmann: US 3,502,763 / 1970, US 3,509,009 / 1970 E.J. Dobo: US 3,542,615 / 1970 O. Dorscher: US 3,692,618 / 1972 W.G. Vosburgh: US 3,368,934 / 1968, US 3,459,627 / 1969 C. Harmon: CA 803,714 / 1969 D. C. Cumbers: GB 1,245,088 / 1971/12 / R.E. Kozulla: US 5,281,378 / 1994 R. J. Coffin, R.K. Gupta: FIA 943072 / 23.06.94 FIA 942889 / 16.06.94 / 13 / S. Piccarolo: J. Macromol. Sci., Phys. , B31 (4), 1992, 501-511 S. Piccarolo, M. Sain, V. Brucato, G. Titomanlio: J. Appl. Polym. Sci., 46, 1992, 625-634 / 14 / B. von Falkai:

Synthesefasern, Verlag Chemie, Weinheim, 1981, 42-43 E. W. Fischer:

Colloid-Z.u.Z. Polymer, B231, 458-503, 1967

Claims (8)

101087 Patented suction A method for controlling the strength properties of a nonwo-5 ven product of a thermosetting process of a fiber gauze formed by synthetic fibers, especially polypropylene fibers, the strength properties of the obtained nonwoven fabric are adjusted as a function of the bonding temperature, the speed of the gauze web and the structural factors of the fiber under the control of the following adjustment equation φ = cx T2 x exp [-E / RT] = 15. V "x exp [-aX] x Cj x T2 x exp (-E / RT] = v“ x exp [-a, fav] x C2 x T2 x exp [-E / RT], where φ denotes the product fabric strength is the tensile strength (σ, N / 50 mm) and elongation (e,%), 20. is the mechanical tensile ratio in the manufacture of the fiber, fav is the average chain orientation of the fibrous polymer structure, v (m / min) is the speed of the gauze web, T ( K) is the absolute temperature, R (cal-joule / ° K * mol) is the general gas constant, E (cal-joule / mol) is the experimentally determined activation energy, 25 c, n, a and a are the experimentally determined constant terms and where E includes the bonding pressure as a parameter and c contains, in addition to the pressure, the activation energy, the temperature difference between the rollers in the roll bonding, the crystalline lamellar thickness of the fiber-polymer structure, the spinning process cable tension, the gauze weight, b the control equation decreases as a function of temperature , get old simulating a similar equation of control equation, i.e., of the form φ = c 'x T2 x exp [E' / RT] where c ', T, E' and R correspond to the terms c, T, E and R before 101087; and the point of intersection of the control equations is the maximum value of the control technical property of the nonwoven fabric and the corresponding temperature, S c. the maximum value of the control strength property is a function of the crystalline lamellar thickness (Dj, Ä) of the fibrous polymer structure, of the form σ ,, ^ (e ^) = Cj x Dj · "1, i.e. the maximum value of the bond strength is adjusted by adjusting the crystalline lamellar thickness of the fiber, The Lorenz-corrected crystalline lamellar thickness varies between, Dz = 20-70 k and the exponent value n, = 0.85 ± 0.15, d. The temperature corresponding to the maximum value of the control technical strength property is a function of the crystalline lamellar thickness of the fiber polymer structure, shape = T - c4 Dz ', i.e. the bonding temperature corresponding to the maximum value of the bond strength, is controlled by adjusting the crystalline lamellar thickness of the fiber, in the operating range where the Lorenz-corrected crystalline lamellar thickness varies between, Dz = 20-70 Å, 20e, where thermal bonding is performed on a fiber-by-fiber basis. thermomechanical shrinkage of the fiber and at the same time 1a the disorientation of the molecular chains of the fiber polymer begins and where the subregions of the fiber matrix. melting point decreases linearly as a function of the inverse of the crystalline lamellar thickness passing through the melting point of the polymer, 30 f. and the activation energy values (E) of the control equations corresponding to the temperature ranges below and above the maximum point of the strength values and the pre-exponential factors In c = -c5E to c6, where c5 and c6 are experimentally determinable 35 constant terms. Control method according to Claim 1, characterized in that the maximum value of the thermal bonding strength is adjusted 101087 as a function of the mechanical draw ratio, X, of the fiber production and thus also as a function of the chain orientation of the fiber structure. Method according to Claim 1, characterized in that, when bonding the one-component fibers, the desired fiber-specific thermal bonding strengths lower than the spinning fibers are achieved by adjusting the mechanical tensile ratio of the fiber in the range, X> 1.0. 10 The control method according to claim 1 a) and b), wherein the strength properties of the nonwoven fabric obtained in thermal bonding are controlled by a control equation including bonding temperature, gauze web speed and mechanical draw ratio of fiber 15, characterized in that a. : 20 gauze weight (w): w = 15-30 g / m2 line pressure between binding rollers (p): p = 50-75 N / mm difference between binding roller temperatures (ϋ): A & = 2-15 ° c spinning cable tension (SLT): SLT = 300-3000 μΝ / filament 25 b. The speed (v) of the gauze web varies in the range: v = 20-150 m / min. with the corresponding velocity exponent (n) varying in the single component fiber range: n = 1.0-1.6 30 c. the mechanical tensile ratio (X) of the fiber tension varies in the range X = 1.5, with the corresponding constant coefficient (a) varying with different polymer grades before the maximum of the strength values in the range: a = 0.75-1.25 and after the maximum in the range: a = 0.40-1.25 35 d. the bonding temperature (T) of the fiber gauze varies in the range: T = 375-450 K 101087 e. for the stabilized fiber structure, at line pressure: p = 60 N / mm, before the maximum of the strength values, the value of the thermal bonding activation energy (E) is: E = 39 ± 4 kcal / mol; this value decreases between: (1-0.25) x E, fiber structure error-S as the states increase; after the maximum of the strength values, as the amount of melt increases, the value of the activation energy varies between: (0.2-0.5) x E, where the lowest value corresponds to the activation energy of the polymer viscose flow 10 f. the dependence function between the activation energy values and the pre-exponential terms of the control equation the values of the standard factors are: cs = 1,160 ± 0.010 C6 = 8,400 ± 0.200 15 The control method according to claim 1, c, d and e, wherein the strength properties of the thermally bonded nonwoven fabric are adjusted by adjusting the crystalline lamellar thickness of the spun fiber polymer structure, i.e., the product of the long identity period and crystallinity degree fraction of the polymer structure, Dz = 20- 70 k, characterized in that a. In order to achieve the desired degree of crystallinity (fc), conventional air quenching of the spinning fiber is performed so that the quenching rate (T) of the polymer is kept close to the temperature corresponding to its crystallization rate (Tc, max, K) (Tc, max = 0.8 x Tmp) to give, as a linear function of the logarithm of the quench rate, the desired crystalline-autumn degrees fe "<0.2; T *,> 100 ° C / s; phases: smectic + amorphous fc: 0.2-0 , 4, 10 ° C / s <Τ, ο <100 ° C / s, phases: smectic + monoclinic + amorphous 35 fc: 0.4-0.6, - T90 <10eC / s, phases: monoclinic + amorphous b achieving the desired degree of crystallinity (fj For example, conventional air quenching of the spinning fiber is performed by quenching the spinning fiber at a rate of 10 ° C / s <<100 ° C / s to form a 3-phase equilibrium and a corresponding degree of crystallinity, and the final desired degree of crystallinity 5 is obtained by annealing the fiber to the Avram growth equation. at a temperature indicated in the range of 60 to 110 ° C within the delay time determined by the line speed. c. in order to achieve a long identity period of the desired spinning fiber polymer matrix in the range, Lz = 90 k to 160 k, the spinning fiber is air-quenched in a manner known per se, using the spinning melt subcooling as the only parameter of the period length, in the temperature range, ΰ = 175-110 ° C. 15 d. to achieve a long identity period of the desired spinning fiber polymer matrix in the range, Lz = 90-160 Å, quenching the spinning melt in the 2-phase range: smectic + amorphous, and annealing the fiber in the temperature range controlled by the measured long period temperature, 20 ϋ = 25-135 ° C, to achieve the final desired period length. A method of adjusting the thermal bonding strength of a fibrous gauze formed by skin-core structured fibers according to claim 1, characterized in that a. The bonding is performed under the control equation in a temperature range exceeding the melting range of the shell layer, 30b. chain orientation: using a corresponding draw ratio and thermally stabilized at temperatures below the melting temperature of the shell layer. 35 A method for controlling the thermal bonding strength of a fibrous gauze formed by skin-core structured polyethylene / polypropylene or / polyester fibers according to claim 1, characterized in that a. polyethylene grades having a weight-average molecular weight and dispersion ranging from Mw = 25,000 to 60,000 and D = 2.5 to 6.0. 10 A method for controlling the thermosetting strength of a fibrous gauze according to claim 1, characterized in that a. The bonding temperature of the fibers used in the hot air and / or furnace bonding of the fibrous gauze is reduced by irradiating the fibers with gamma rays before bonding in spinning (XK = 20 90-1600) and / or thereafter mechanically so that the average chain orientation of the product fiber is in the range, fav = 0.4-0.8. 101087