CN1330741A - Softened comminution pulp - Google Patents

Abstract

The present invention relates to processes for softening cellulose pulp using chemical softening agents or debonders, which include compositions comprising lower alkyl acid esters or cyclic esters of polyhydroxy compounds, without adversely affecting the absorbency of the cellulose fiber products thereof, and products thereof. The process of the invention may also be used in combination with plasticizing agents for cellulose such as glycerol, mono- and di-saccharides, glycols, and oligomers thereof. The process of the invention provides cellulosic fiber which is easier to fluff (refiberize) and to subsequently densify airlaid pads formed from the resulting individualized fibers, without adversely affecting absorbency.

Description

Softening comminution pulp

Related application

The application has required the interests in the U.S. Provisional Patent Application 60/112,887 of submission on December 18th, 1998.

The field of the invention

The present invention relates to adopt chemical softener, the method of the plain paper pulp of softening fibre, this softening agent comprises the composition and the polyhydroxy official energy plasticizer of detackifier such as low alkyl group acid esters that contains polyol or cyclic ester, the product that obtains thus, and similar substance.

Background of the present invention

High-tech absorbent commodity is such as senior baby diaper, adult incontinence devices, and sanltary towel all is by making based on the absorption of cellulose fibre fur nuclear usually, this nuclear is positioned at a supernatant liquid infiltration thin slice and low-density obtains or wash-prime coat below.Obtain layer allow the interim storage of liquid and liquid clog-free by up to absorb nuclear simultaneously it also as obstacle to stop the anti-skin that flows back to the user of liquid.The impermeable support thin slice of liquid, plastic substance is normally also provided to hold absorbed liquid and to prevent that it from seeing through to absorb nuclear and the people's that wears absorbent commodity of making dirty underwear.Obtain layer and generally include the cellulosic fluff of sclerosis chemically or the synthetic fiber of bonding, wherein fiber is with thermoplastic binder fiber or powder, or by using latex adhesive to be bonded together.

The absorption nuclear of these absorbent commodities generally includes the wood pulp of the defiberization that contains or do not contain superabsorbent polymer particles.Absorb nuclear moulding on the mat forming unit of the converter on the conveyer belt (carrier tissue) usually, be beneficial to processing.Some absorb nuclear forming units and have vertical resolution, wherein another discrete fur layer can be placed on initial based on the absorbed layer of fur to form a kind of multilayer absorbing structure.In these absorbing structures, initial layer can contain superabsorbent polymer particles.The example of the absorbing structure that routine is made is included in United States Patent (USP) 5,009,650; 5,378,528; 5,128,082; 5,607,414; 5,147,343; 5,149,335; 5,522,810; 5,041,104; 5,176,668; 5,389,181; With 4,596, those of explanation in 567.

The production of disposable absorptive health product, particularly diaper and adult incontinence products carry out on continuous production line usually, and wherein the cellulosic fluff absorbent material provides with the paper pulp roll form of pulverizing.Traditional wet shop technology is adopted in the production of paper pulp, and wherein the paper pulp thin slice is unfolded and is sent in hammer-mill or the similar mechanical device so that the cellulose fibre in the thin slice is separated into cellulosic fluff.Before hammer-mill, can have also and can not have drying stage, decide on the skilled craftsman's that uses the inventive method needs.Then fur is transferred to shaping area, will be carried out the gas shop to it by amount that requires according to final products and shape at there.

For the softening product that is made into thin slice to pulverize fully, adopt cationic surfactant to come association between devillicate usually, to make a soft and weak sheet product as detackifier.United States Patent (USP) 4,432,833; The example of detackifier is disclosed in 4,425,186 and 5,776,308.So a total shortcoming of tradition CATION detackifier is to lose because of the wettable and the absorbability of the long relatively comminution pulp of alkyl chain of cationic surfactant.So blocking-up hydrogen binding site can the softening pulp thin slice it can more easily be pulverized and be fiber independently.Detackifier also helps to form senior, low-density gas shop structure, and this structure can be resisted permanent densification, because interfibrous hydrogen bond is intercepted by the detackifier molecule.Therefore, it helps producing the comminution pulp product, and does not lose wettable and absorbability, and this product is easy to densification to be used for final gas shop or textile product.

Cellulosic plasticizer, they can join in the pulp slurry before forming wet shop thin slice, also can be used for softening pulp, though they are had an effect with the mechanism that differs from detackifier.Plasticizer is had an effect to cellulosic molecule between fiber, thereby makes unformed area submissive or softening.The gained fiber has soft characteristic.Not hard because of plasticized fiber, be easy to densification so compared with the fiber of handling without plasticizer by comminution pulp.

Plasticizer comprises that polyalcohol is such as glycerine; Low molecular weight polyglycols such as polyethylene glycol and polypropylene glycol; And other polyol.United States Patent (USP) 4,098,996, United States Patent (USP) 5,547,541 and United States Patent (USP) 4,731,269 be illustrated and provide example to these and other plasticizer.Ammoniacal liquor, urea, and alkylamine to be used for the plasticising woodwork also very well-known, these woodworks comprise that mainly cellulose (sees the forest product magazine 5 (6): 413,1955 of A.J.Stamm.

Plasticising becomes different the densification of the gas shop adhesive-bonded fabric of being made by processed paper pulp after pulverizing.The method of a softening fibre promotor composition, it can be effectively to the paper pulp fiber unsticking with abundant pulverizing, thereby but fibration and densification are in succession become different do not reduce wettable, will be very useful, but also not have in the prior art.

The present invention's general introduction

The invention provides a kind of new method, and by it and product, be used for by using a novel chemical softener combination, it not only contains detackifier but also contains plasticizer, comes the plain paper pulp of softening fibre.This softening processing makes common fur paper pulp thin slice be converted into the softening thin slice that is formed by flexible fibre, the mutual compatibility of these flexible fibres very little (such as, paper pulp plasticising or unsticking).Therefore, formed paper pulp not only is easy to into fur (fibration again) but also is easy to densification subsequently and changes into the gas place mat, and these gas place mats are formed by pulverized defibre.In addition, softening method of the present invention is without detriment to the absorbability and the wettable of cellulose fibre.

Detackifier but also plasticizer are not only adopted in practice of the present invention, have reduced that widely the paper pulp fiber thin slice is converted into the absorbent products energy needed.Because the energy that needs is lower, output is higher, and has reduced the equipment abrasion, makes production cost of products so method of the present invention has reduced by Fibrotic comminution pulp again.These are surprising and pennies from heavens of the present invention, adopt traditional detackifier or plasticizer softening pulp can not obtain these benefits in the past separately.

In one embodiment, the invention provides one and be used for the plain process of pulp of softening fibre, it comprises the step that paper pulp is contacted with the aqueous solution that contains detackifier and plasticizer combinations.

Another embodiment of the invention provides a kind of novel detackifier, propylene carbonate, and it can be used alone as detackifier, or uses with the plain paper pulp of softening fibre with the plasticizer of the process according to the present invention.

The softening pulp that is used for absorbent products that the present invention also provides a kind of process according to the present invention to make.

The simple declaration of figure

Fig. 1 is a curve map, shows with the detackifier that accounts for solution 5,10 and 15% weight--propylene carbonate and glycerol triacetate the variation of the TENSILE STRENGTH of the paper pulp thin slice of handling.

Fig. 2 is a curve map, only shows the paper pulp thin slice of being handled by detackifier, only the paper pulp thin slice of being handled by plasticizer and by the variation of the TENSILE STRENGTH of the paper pulp thin slice of the mixture process of plasticizer and detackifier.Adopt propylene carbonate, glucose is respectively as detackifier and plasticizer.

Fig. 3 is a curve map, only shows by detackifier to handle, and is only handled by plasticizer and by the variation of the TENSILE STRENGTH of the fiber of the mixture process of plasticizer and detackifier.Adopt propylene carbonate, glycerine is respectively as detackifier and plasticizer.

Detailed description of the present invention

All references that the application quotes are all with reference to incorporating into. When there is contradiction in the reference of the disclosed content of the application and Insert Here, comprise term contradiction, all be as the criterion with the application.

Picture is used herein, softening agent, compound or composition comprise be selected from detackifier and plasticizer any can softening fibre the compound of element paper pulp. By the paper pulp of " modification ", once processed with softening agent or contacted with softening agent.

The detackifier that is used for the softening fibre cellulose fiber that the present invention is used, low alkyl group acid esters or cyclic ester except polyol outside alkyl ether and the aryl oxide, also comprise any traditional cation detackifier well known in the prior art.

The preferred detackifier of the present invention comprises propylene carbonate, glycerol triacetate, propylene glycol diacetate, 2-phenoxetol, and the mixture of these materials.

Propylene carbonate, the cyclic ester of propane diols and carbonic acid are the sprotic high boiling solvents of having of polarity, it extensively is used as the solvent of multiple polymers, (for example, United States Patent (USP) 5,580,922,5,554,657 and 5,629,277). The inventor is surprised to find that propylene carbonate also is a kind of effective detackifier of cellulose fibre, and it does not have the impact of thing followed minor face to wettable and the absorbability that the thin slice gas that is obtained by pulp treatment spreads product. The non-cyclic ester that removes sticking effect and polyol of propylene carbonate, such as glycerol triacetate, similar.

In one embodiment, a kind of detackifier of the present invention and known plasticizer are united and are used for the softening fibre element.The plasticizer that the present invention uses comprises polyol, low-grade alkylamine and diamine, and urea, and have substituent urea, such as tatramethylol urea, single-and two-carbohydrate, glycol, and their oligomer.Preferred plasticizer of the present invention comprises glucose, glycerine, and polyethylene oxide.

A preferred detackifier/plasticizer combinations is propylene carbonate and glycerine or other polyol, glycerol triacetate and glycerine, and propylene carbonate and glucose.

Detackifier of the present invention and plasticizer can have been bought.Propylene carbonate can (Houston TX) obtains in a large number from Huntsman company; Glycerol triacetate and diacetate glycol ester can (Kingsport TN) obtains from Eastman chemical company; Glycerine can (Columbus OH) obtains from Ashland chemical company; And glucose can (Gardena CA) obtains from Spectrum Bulk chemical company.

During use, softening compositio, they can both contain also plasticizer-containing of detackifier, can be effectively to the fiber unsticking in the paper pulp thin slice reducing interfibrous association, and without detriment to follow-up densification process.Will make the TENSILE STRENGTH of processed paper pulp thin slice lower like this (go glue sign) and make to pulverize to fiber independently and become different.The plasticizer of softening compositio infiltrates through in the fiber and inner it to be softened and plasticising.Will obtain an absorbent products that is easy to the drying and moulding of densification like this.

In the laboratory, it is very convenient simply to flood the comminution pulp thin slice with the softening Treatment Solution of water-based, and the practice is that dipping blots then gently earlier.In the production process of reality, can be before thin slice enters drying stage or will soften additive later on and spray or otherwise be applied on the online paper pulp thin slice.Also can before thin slice forms, tenderising soln be added in the pulp slurry.On the production line of gas shop, when the paper pulp thin slice launches and delivers to hammer-mill or other disintegrating apparatus, tenderising soln is sprayed or otherwise be applied on the paper pulp thin slice.

The amount that is added to the tenderising soln on the paper pulp thin slice depends on the concentration and the product desired destination concentration of additive in the treatment fluid.Processing time inessential (for example, it does not influence the softening performance of the paper pulp of handling), and it can be in several seconds to several days scope.

Treatment Solution can comprise detackifier and the plasticizer of 2-99 weight %.The preferred concentration of solution is in the scope of 3-7 weight %.The process of sheeting extension test

Adopt Thwing Albert intelligence II tester for elongation, model 1450-24-A, the fracture strength of the laminar cellulose bar that test is dry.TENSILE STRENGTH is with pound/inch sample width gauge.Operating direction along thin slice is cut into 4.5 inches bars that multiply by 1 inch with sample.If fracture strength surpasses 100 pounds/inch, the width of sample adopts 1.5 centimetres when testing so.Extension test carries out in the laboratory that temperature and humidity is controlled, and temperature is that 23 ± 1 ℃ (73.4 ± 2) and relative humidity are 50 ± 5%, and before the test with sample balance at least two hours.Carry out twice or three times test, and in addition average to the result.

Below can be used for measuring the performance of the plain paper pulp of gained softening fibre.Measure the process of separation energy

The comminution pulp thin slice that to make with conventional wet shop technology by Buceys industrial group, optional dry again with softening additive treating, and to be cut into along operating direction be 30 inches 2 inches * 30 inches bar.Comminution pulp usually quantitatively be about 700 restrain/square metre.Write down the actual weight of each bar and respectively these are sent into the Kamas laboratory hammer mill, Kamas industry AB model KVARNH01 separates.This hammer-mill has one to be of a size of the sieve of 16-17 millimeter and to be under the condition of 8 feet per minute clocks with the speed operation of 400rpm at feeding speed.Measure and separate required energy consumption and be typically expressed as KWH/ ton (kilowatt hour/ton paper pulp).Moisture or even relative humidity remaining in the paper pulp thin slice can both influence separation energy.Therefore, when measuring each sample, all the reference bar that is untreated is tested to obtain a benchmark and compared.The result of any given day just can be scaled the value of other any given day by the ratio that multiply by reference batten separation energy so.With the absorbability of doing test gas felt, the preparation process of the sample of intensity and liquid conveying function

The cellulose fibre that uses in the tested gas felt pan is by never making through the cellulose pulp of super-dry of obtaining from Buckeye industrial group, and or with softening agent of the present invention handle or with laboratory paper machine (the dynamic molding machine of Alimand) be shaped to 700 grams/square metre thin slice after no longer processing.This machine is ejected into the dilution slurries of paper pulp fiber on the high speed rotating drum and therefore forms a thin slice of 8.5 inches * 35 inches with real operating direction.Dry laminar paper pulp can be by being cut into paper pulp 2 inches * 30 inches bar, and be converted into the gas felt that does not contain a large amount of fibrous masss.Batten is sent into Kamas industry AB model KVARN H 01 laboratory hammer mill respectively to produce the fur of homogeneous.

Adopt the laboratory-scale mat producing machine, its one-tenth pad method is identical with commercial one-tenth pad method, and the fur gas with dry homogeneous under controling environment is paved into the gas felt pan.In order to overcome the influence that separates comminution pulp under without the environment of condition control and mat to be exposed down controling environment, mat can be placed in mat producing machine 4-5 minute, the air that control this moment passes mat.In addition, to have overcome the used compressed air relative humidity of system pad be not 50% and the influence that may cause to this process.

The tissue paper flaggy that will be of a size of 14-1/2 inch * 14-1/2 inch is put on the moulding sieve of mat producing machine.These tissue papers cover the moulding sieve fully and turn up on the limit.These tissue papers are represented the bottom side of gas shop gas felt pan.An amount of fur sample is added mat producing machine with the quarter increment, and mat revolves and turn 90 degrees to form the mat of homogeneous between every part.After being added to fur on the gas felt pan of gas shop, the moulding sieve of gas felt pan being arranged above removing, and transfer to lightly on the even surface.With another one cover tissue paper perform mark with the upside that marks gas shop gas felt pan and with this tissue paper be put into mat above.A weight that is of a size of 14 inches * 14 inches is put on the mat in the mode of not disturbing the gas felt pan to form.Weight minimum maintenance 5 minutes on the gas felt pan, and then remove carefully.Cut out plate with normal paper and remove about 12-3/4 inch * 12-3/4 inch from every limit, thereby mat is cut to 12-3/4 inch * 12-3/4 inch square.Mat is cut into side's pad that 9 sizes are 4-1/4 inch * 4-1/4 inch.Then gas is spread felt pan be placed on a temperature be 23 ± 1 ℃ (73.4 ± 2) and relative humidity be 50 ± 5% place when needs are tested till.Carefully remove the covering tissue paper on 4-1/4 inch * 4-1/4 inch pad, and mat is put on the latter half of aluminium compressing tablet.This compressing tablet is made up of two 6 inches * 6 inches * 1 inch aluminium block.6 inches * 6 inches faces of each aluminium block are processed into quite flat surface.Alignment pin is fixed near two angles of a plate.On another plate, there is corresponding hole to be used to accept pin.The first half of compressing tablet is placed on the mat that will be pressed and with whole compressing tablet and is placed on (model: 16600-224) on the Carver hydraulic press.Suppress each mat to produce desirable density with suitable pressure.Because the size of mat increases because of compacting, so mat is cut to 4 inches * 4 inches and weigh.Waited for for 120 seconds for the bounce-back that lags behind, measure the thickness of each mat then.Calculate the density of mat then according to following formula:

The density of one the 4 inches * 4 inches pads (test process of gram/cc)=0.000379 * weight (gram)/thickness (inch) instillation (drip) ability

In order to show according to the present invention the fluid delivery capability of the absorbing structure of making by the cellulose fibre of handling through detackifier and/or plasticizer, prepare the gas felt pan according to said process.The fluid delivery capability of each gas felt pan is by measuring the instillation ability, is expressed as cellulosic gram number in the milliliter number/gas felt pan of liquid, and tested, and do not cover tissue paper during test on the mat.By 9 gram NaCl being dissolved in the 991 gram distilled water and with 0.9% NaCl simulation urine.With pack into a buret and the flow velocity of pipette is adjusted to discharges 2 milliliters of urine each second of this salting liquid.Release end on the buret tap is perpendicular to the cube of being made by 0.5 inch silk screen and 1 inch place placed on it.This cube is placed in the dish to accept excessive fluid.Cubical end face remains level.

Press to after the desirable density, immediately mat is put on the cube so that the fluid impact point is in the cross spider position.Simultaneously the tap of buret is opened and started timer.Experimental Flowing Object drips to the centre of mat with the speed of control.When being discharged on the plate by mat, first drop of liquid stops timer.Write down first drop of liquid by the required time of mat.The mat that will wet is removed and is thrown away from cube.The cube bone dry is also put back in the dish again.Repeat said process with two other gas felt pan again, the weight of these two mats, density and composition are identical with first.Write down in these three mats each weight, density and time.Calculate the instillation ability of each mat and average according to following formula with remaining:

The process of weight (gram) total absorptivity of instillation ability (liquid milliliter number/gram sample)=time (second) * 2/4 inch * 4 inches mats

In order to show the absorbability of the absorbing structure of making by the cellulose fibre of handling through softening agent according to the present invention, prepare the gas felt pan according to said process.Measure the absorbability of the gas felt pan that does not cover tissue paper.With one 4 inches * 4 inches gas felt pan, nominally be 300 grams/square metre and density be 0.2 gram/cc, be put into plastics and claim on the price fixing and weigh.Mat and plate are put on the sloping platform of one 60 degree.NaCl dipping mat with 0.9%.Excessive liquid drains off and it is removed with blotting paper.The mat of plate and dipping is weighed.

Total absorbability is counted:

The process of absorbability (gram/gram)=(weight in wet base-dry weight)/dry weight rupture strength experiment

In order to show the rupture strength of the absorbing structure of being made by the cellulose fibre of handling through detackifier according to the present invention, the method according to this invention prepares gas shop gas felt pan.Preparation is used as the gas felt pan of reference pad according to said process, and they contain cellulose fibre or the undressed cellulose fibre that glues.Arrive the rupture strength that the needed power in without hindrance force on the mat that does not cover tissue paper is evaluated each mat by measuring spherical penetrator on traditional tensile test device.

Adopt Thwing Albert intelligence II tester for elongation to measure the rupture strength of gas felt pan.Tester for elongation comprises that a jig platform and clamping plate are used for the test mat is fixed on horizontal level between jig platform and the clamping plate.Have corresponding hole to be used to accept spherical penetrator on jig platform and the clamping plate, this penetrator be placed in the hole directly over.Tester for elongation is installed and receives on the gram battery to compress mode, it monitors any resistance that spherical penetrator ran into of 1.5 centimetres of diameters.

After being depressed into the density of 0.2 gram/cc, mat is put on the hole of jig platform immediately, and clamps mat safely so that mat is fixed on the appropriate location with clamping plate.Start intelligent machine, crosshead is made as downward operation, speed is 0.5 inch per minute clock or 1.27 cm per minute.When spherical penetrator moves downward and touches mat, will demonstrate ever-increasing power continuously on the monitor.Penetrator continues to see through mat fully till arriving without hindrance force, and it is exactly that mat is when breaking usually.At this point, the crosshead preliminary examination position of upwards rebounding automatically.Maximum, force value on the record intelligent surveillance device.Repeat twice of this process with new gas felt pan.With the value of three mats in addition mean deviation be unit record maximum, force value with the gram.The process of vertical wicking (wicking) speed

The gas felt pan is closely knit to 0.1 gram/cc, accurately be cut to 4 inches * 4 inches, and correctly be installed between the plastic plate that has the electronics humidity sensor.Sample clamp than salt water storage tank low 1/4 inch and when liquid rise on the storage tank 1/4 inch and when touching low row's sensor timer start automatically.When upper electrode (higher 1.5 inches than first row) was run in the liquid forward position of moving, timer stopped automatically.The result is in cel.The process of laminar cellulose pulp inclination wicking rate

In this experiment, a plastic plate that has an inch level scale is placed on the direction that becomes miter angle with vertical direction the storage tank top of dying red 0.9% NaCl with food coloring commonly used is housed.Paper pulp thin slice (by the densification of gas place mat) is put on the plate of inclination, 1/4 inch in storage tank, and start stopwatch.The forward position of record liquid upwards arrives 3.5 inches time.With the result is that unit lists in the table with the inch per second.In this experiment, will in distilled water, soak a night by the laminar cellulose pulp that Buckeye industrial group obtains with paper pulp rehydration.The paper pulp of swelling is anhydrated by mediating rod on the felt of paper-making machine, then this paper pulp is sprayed with softening agent solution.By the amount and the humidification amount of the dry pulp in the processing thin slice that calculates, can calculate the percetage by weight (" % increment ") of increase.In following table, PC is a propylene carbonate, and G is a glycerine.The inclination wicking rate is not subjected to the influence that softening agent is handled when arbitrary density.The process of separative efficiency (DE)

This method is used to measure the separation of comminution pulp or becomes the capillary effect rate.The amount of the separated paper pulp of this measuring, the enough fibrations of these separated paper pulp are passed through 14-mesh sieve (1.4 millimeters holes) with activation.With fur,, accurately be divided into weight and be two parts of 5.00 grams for example by Kamas laboratory hammer mill gained.Portion is transferred on 14-mesh sieve of vacuum-pneumatic separation chamber.This device comprises that the diameter of a standard is 8 inches a Tyler sieve, and this sieve has a transparent plastic cover that is loaded on the transparent plastic drum, and this cylinder has an outlet to link to each other with vacuum cleaner, and another links to each other with pressure gauge.This transparent plastic chamber also has one to be furnished with the pneumatic inlet that is flexible coupling, thereby guiding compressed air stream fully stirs the fur sample, and this can observe by transparent plastic cover.After shaking 2 minutes simultaneously with compressed air, remove the separated paper pulp that under 3 centimetres of Hg post vacuums, sees through 14-mesh sieve, just can obtain staying the part on the sieve again.Fur with another 5.00 grams partly repeats this process.To obtain again from the sieve these two partially mixed and weigh.The weight of separated fur is that 10 grams deduct the thing useless that obtained by 14-mesh sieve or the weight of fibrous mass.

Separative efficiency=(weight of 10 gram-not separated furs) * 100/10 gram

Provide following examples with further explanation the present invention, scope of the present invention will only be limited on book.

Embodiment

Because the natural residual moisture of cellulose pulp is proportional with its temperature and the relative humidity of environment of storage, and the degree of the drying condition that has just stood with fiber is proportional, so adopted a reference paper pulp batten in this experiment.So under study for action just can be by obtaining an initial weight and adopt a reference batten (handling) without softening, and calculate the combination degree that the extent of reaction in the paper pulp or chemical tendering are handled.The reference batten is used for measuring the water content of original material so that measure the actual weightening finish of treated sample.

In following examples,, can calculate the combination degree of softening agent, i.e. the percentage of additive in processed thin slice by contrast treated sample and the reference batten of crossing and stand the drying condition as experiment is handled through deionized water dipping.The weight difference of initial reference and dry reference is used for calculating the actual paper pulp weight of initial sample.Final per cent additive is that the final dry weight of processed thin slice and the difference of the initial dry weight through calibrating are removed final dry weight.In addition, the TENSILE STRENGTH of the paper pulp thin slice that the method according to this invention is handled, with ft lbf/inch width gauge, can calculate by traditional method.

If the softening agent of dissolving is absorbed soon by paper pulp, so absorbed solution may no longer contain these reagent, therefore causes the height of planting the expection of negative quantity ratio of softening agent in the final pulp product.On the contrary, if moisture is the stronger attraction of paper pulp, just may be rich in softening agent in the so excessive solution.If this softening agent is a wetting agent, moisture residual in the so processed paper pulp just may so just cause a paper pulp weightening finish that is summed up as the too high report of handling chemicals mistakenly than the moisture height in the paper pulp that is exposed to pure water.Therefore, in following examples, suppose that solution and the initial soln retained in the wet pulp contain same softening agent.

Embodiment 1

In this experiment, containing the aqueous solution dipping of 5% softening agent, softening agent and is removed excessive solution as shown in Table by blotting at once with the southern softwood kraft paper pulp thin slice of 1.5 * 6.0 inches (about 4.5 gram).Batten is following dry 60 minutes at 109 ℃.

Employing is estimated Fibrotic easness in fixing speed and the laboratory blender moved under the time to 0.7 gram modified pulp thin slice, it show clearly paper pulp fiber go sticking and softening.When opening fully, fur can be accumulated in top away from the blender of blade by the blade that compresses (impacting) blender.With sample furization as far as possible fully in blender, then to be shaped to quantitatively be 390 grams/square metre the mat of 2.25 inches of diameters.With mat in 30 handkerchief/square inches (psi) press 10 seconds and in 60/ square inch press once again after, measure the density of mat.

Compare with undressed sample, slacken thin slice a little with the water treatment meeting separately, but can reduce the density of gas place mat, as shown in table 1.

Through glycerine, a kind of known cellulose plasticizer, the paper pulp of processing has the TENSILE STRENGTH that has reduced, show obtained softening.Yet this paper pulp is difficult to fibration in blender, because fibration needs second more than 20.The mat that the fiber that compacting is handled by glycerine obtains can produce the mat of a densification, and this is desired to plasticized fibre.

The paper pulp thin slice of handling with glycerol triacetate or propylene carbonate (PC) has low TENSILE STRENGTH and furization easily, and the two all is that the paper pulp thin slice fully goes the confirmation of gluing.

Table 1: the dipping of paper pulp thin slice

Pulp processing	Increment percentage	TENSILE STRENGTH (pound/inch)	Blender fibration (second)	Gas shop density (gram/cc)
					Be untreated	????0	????107.1	????20+	????0.24
Water	????0	????94.9	????20+	????0.21
					Glycerine	????6.5	????68.2	????20+	????0.26
Propylene carbonate	????5.0	????52.8	????10	????0.23
					Glycerol triacetate	????5.4	????45.0	????10	????0.21

In embodiment (2-5), comminution pulp thin slice (Foley fur; Buckeye industrial group) is cut into 1.5 inches * 6.0 inches batten along operating direction.Batten is weighed into immediate milligram (about 4.5 grams) then as each embodiment is described, uses softening treatment fluid dipping.Blot excessive treatment fluid, the weighing of sheets that will wet then is put in the laboratory convection oven and removes moisture under different temperatures.

The mixture of embodiment 2 plasticizer and plasticizer and detackifier

With various plasticizer and the plasticizer that is mixed with water-based propylene carbonate (detackifier), as shown in table 2, the pulp treatment strip of foil, as shown in table 2.Flood the paper pulp thin slice respectively and contain each component with 5% solution of each softening component and be 5% solution impregnation paper pulp thin slice with one.The 5%th, the concentration of solution.Table 2 has shown the amount of additive with the percentage form that accounts for output aggregate.Thin slice is following dry 60 minutes in 109 ℃ in convection oven.

Go sticking effect, represent by the increment percentage of absorbed treatment fluid, almost be unite use propylene carbonate and glucose add and.These softening agents are used as the detackifier of paper pulp thin slice together than using each much effective respectively.

TENSILE STRENGTH through the sample of glycerine and propylene carbonate Combined Treatment is lower slightly than the mean level of the sample of handling respectively through them.

Through urea, the cellulose plasticizer that another is known, the sample of processing does not show and significantly goes sticking activity.Through the sample of urea and propylene carbonate Combined Treatment, the TENSILE STRENGTH of demonstration is consistent with the mean level of the sample of handling respectively through these reagent.

Table 2: plasticizer, detackifier, and composition thereof

Pulp processing	Additive accounts for the percentage of product	TENSILE STRENGTH (pound/inch)	Average tensile strength (pound/inch)
				The paper pulp thin slice is untreated	????0	????107.1
Glucose	????7.1	????86.5
				Propylene carbonate	????5.0	????52.8
Glucose and propylene carbonate	????11.5	????43.4	????65
				Glycerine	????6.2	????69.2
Glycerine and propylene carbonate	????8.1	????57.7	????61
				Urea	????6.0	????109.9
Urea and propylene carbonate	????7.6	????81.6	????81.4

Embodiment 3-temperature experiment

Baking temperature handles the effect of fiber for propylene carbonate or modification (softening) degree of fiber does not have the uniformity influence.Propylene carbonate aqueous solution dipping paper pulp thin slice with 5% is also dry, as shown in table 3 under different temperature.The recruitment that the softening efficient of handling is expressed as final dry weight accounts for the percentage that is added to the propylene carbonate total amount on the paper pulp in the moistening stage.The table of degree of handling is shown the percetage by weight of final products.

Table 3: baking temperature research

Temperature ℃	Efficient %	The % propylene carbonate
			????88	????62.3	????4.8
????100	????56.4	????4.4
			????125	????59.4	????4.5
????135	????60.1	????4.4
			????150	????57.8	????4.5

The residual research of embodiment 4-detackifier

Experimentize to measure cellulose pulp retains the organic ester detackifier under different temperatures ability.Softening agent solution impregnation paper pulp thin slice with 5% is also dry in 135 ℃ baking oven.

These result of experiment show the cellulose pulp absorption and retain the limited in one's ability of organic ester detackifier, but this ability is somewhat dependent upon used softening agent and drying condition.The most weightening finish of sample occurs in for the first time and handles.Processing again only can increase a little and remains in unsticking dosage in the paper pulp.When the pulp sample of only handling with glycerol triacetate each handle the back earlier 25 ℃ of dryings then at 109 ℃ when dry, can show higher total augment weight.Total augment weight under these conditions is to handle and then in the twice of 135 ℃ of total augment weights when dry with glycerol triacetate.For the sample of handling with propylene carbonate (PC), temperature is very little to increase heavy influence.

Table 4: detackifier, the processing of continuation

Handle for the first time	Weightening finish %	Handle for the second time	Total augment weight %
				Glycerol triacetate, 135 °	4.2	Glycerol triacetate, 135 °	4.3
Glycerol triacetate, 135 °	4.24	Propylene carbonate, 135 °	5.08
				Propylene carbonate, 135 °	4.4	Propylene carbonate, 135 °	5.2
Propylene carbonate, 135 °	4.5	Glycerol triacetate, 135 °	5.03
				Glycerol triacetate, 25 °	Do not measure	Glycerol triacetate, 109 °	8.48
Propylene carbonate, 25 °	Do not measure	Propylene carbonate, 109 °	4.75

Embodiment 5-detackifier is loaded with

To contain 5,10,15% solution impregnation paper pulp thin slice of glycerol triacetate or propylene carbonate, blot immediately, and in 135 ° convection oven dry 60 minutes.Propylene carbonate can mix with water, can change by the concentration that changes treatment fluid so the initial wet on the paper pulp is loaded with.The solubility of glycerol triacetate in water is limited, so simulate 10 and 15% data point by repeatedly handling with 5% glycerol triacetate.See Table 5 and Fig. 1.Having adopted a reference with water treatment to be used for moisture proofreaies and correct.Final degree of treatment accounts for the mark of final weight in the weightening finish that is caused by detackifier.

As shown in Figure 1, when paper pulp was dried under 135 °, paper pulp absorbed the propylene carbonate or the glycerol triacetate solution of 5% weight that is approximately processed paper pulp.

The effect of 5:135 ° of following detackifier concentration of table

Concentration	The % propylene carbonate	The % glycerol triacetate
			????0	????0	????0
????1	????0.8	????1
			????2.5	????2.6	????2.2
????5	????4.7	????3.4
			????10	????4.7	????4.3
????15	????4.9	????4

Embodiment 6 TENSILE STRENGTH/additive is loaded with

With plasticizer, behind the various dilution dipping paper pulp thin slices of detackifier and 1: 1 mixture thereof, this experiment is tested the TENSILE STRENGTH of paper pulp thin slice as the function of modification degree with TENSILE STRENGTH, is expressed as pound/inch width.Additive is loaded with the percetage by weight that is expressed as final pulp product.To the results are shown in table 6 and draw and be Fig. 2 and Fig. 3.Table 6 comprises three parts: plasticizer, detackifier and both mixtures.The TENSILE STRENGTH of paper pulp thin slice is an indication of sticking effect.Even plasticizer seems to slacken thin slice, but the effect of glycerine is bigger than glucose.Yet and propylene carbonate unites when using, and glucose is more effective than glycerine.As detackifier, loading with of propylene carbonate and glycerol triacetate can reach 5.4% (upper limit of propylene carbonate dosage).Fig. 2 is drawn by the glucose and the propylene carbonate data of table 6, and Fig. 3 is drawn by glycerol triacetate and propylene carbonate data.

Table 6: the TENSILE STRENGTH of loading with the paper pulp thin slice of function as additive

Plasticizer detackifier mixture

The % additive	Glycerine	Glucose		Glycerol triacetate	Propylene carbonate (PC)		PC/ glucose	PC/ glycerine
									????0	?90.2	?90.2		????90.2	????90.2		????90.2	????90.2
????2.2					????65.1
									????2.8				????43.6				????88
????3.7	?69.4
									????4.4		?87		????44.8
????4.6					????51.2
									????5	?70.2				????52.8
????5.4				????45	????44.4			????61.3
									????6.1	?69.2						????54.9
????6.6	?68.2
									????7.1		?86.5
????8.3								????57.7
									????8.5				????31.2
????11.6							????43.4
									????12.1	?47.3
????14.3		?72.6
									????16.7							????29.5

Annotate; Shown in the blank in the table, be not that all prescriptions are all tested under various processing horizontals.

The impregnation process of embodiment 7 paper pulp thin slices

The measurement that stretches is to measure a kind of method that pulp additive goes sticking effect.Another kind to cellulosic fibre material thin slice intrinsic strength is tested the separation energy of grinding for Kamas.In table 7, to the Kamas energy of processed paper pulp, TENSILE STRENGTH, and separative efficiency is measured.By strip being immersed in other solution of branch, blot excess solution, and dry in 109 ° convection oven, thus the dry batten of comminution pulp (Buckeye industrial group) is handled.In table 7, propylene carbonate is abbreviated as PC, and glycerol triacetate is abbreviated as TA, and molecular weight is that 200 polyethylene glycol is abbreviated as E-200.Because separation energy (KE) depends on a lot of variable elements, so a undressed reference paper pulp thin slice is tested with every group of sample.Sample is listed by the order that Kamas can successively decrease.

Table 7: separation energy and TENSILE STRENGTH

Handle	% loads with	KE (kilowatt-hour/ton)	TENSILE STRENGTH (pound/inch)	??DE(％)
					Do not handle	????0	????30.2	????101.3	????89
Water	????0	????27.3	????93.4	????94
					?1.25％PC/E-200	????3.5	????22.9	????49.8	????98
?2.5％PC/E-200	????6.5	????21.0	????45.4	????96
					1.25%TA/ glucose	????3.9	????20.5	????47.8	????97
?1.25％TA/E-200	????3.7	????18.4	????41.7	????97
					?2.5％TA/E-200	????6.4	????16.8	????35.2	????97
2.5%TA/ glucose	????7.4	????16.3	????40.6	????98

Even only can cause also that with water treatment the paper pulp thin slice is stretching, separation energy and separative efficiency aspect significantly slacken.TENSILE STRENGTH through the softening sample thin slice of handling has a relatively large drop than its separation energy.TENSILE STRENGTH and separation energy are directly related.Dense more gained energy of treatment fluid and intensity level are low more.

Embodiment 8-10: the paper pulp thin slice of handling again aquation

The laminar cellulose comminution pulp of Buckeye industrial group is soaked a night so that paper pulp is carried out aquation again in distilled water.The thin slice of swelling is anhydrated on the felt of paper-making machine by mediating rod, and then spray is with softening agent solution.This process is used in two contrived experiments (three ranks and two factors) and two simple experiment (three ranks of a factor) and handles from the analogy method of the paper pulp thin slice of undried as a kind of, and wherein this thin slice need not actual fabrication.Calculated value and wet weightening finish by the dry pulp in the processed thin slice can draw the percetage by weight of increase.In following table, PC is a propylene carbonate, and G is a glycerine.Drying slice is cut into 2 inches * 30 inches along operating direction bar grinds to send into Kamas.Fur sample that will modification in table 8-10 listed experiment be blown into 450 grams/square metre thin slice (handsheet) in, this pad has carried out densification with the Carver press, and in table 8, has passed through inclination wicking and tested (at 45 with vertical direction).By the forward position of liquid upwards reach 3.5 inches required times of distance can calculate speed.The independent additive laboratory report of the contrived experiment of table 9 and table 10 separation energy and to providing the batten latter end of sending into remaining (left-over) in the hammer-mill to carry out extension test.Test separative efficiency and assessed the easness of densification.By fur prepare 450 the gram/square metre the gas felt pan after, at once mat power (312psi) with 5,000 pounds/4 inches * 4 inches pads on the Carver press is suppressed.Measure thickness and calculate actual density.Gained density is high more, and the easy more densification of fiber also keeps fine and close.This is used to survey the existence of cellulose plasticizer.

Table 8: inclination wicking research

Handle	Density (gram/cc)	Su Shuai @3.5 inch (inch per second)
			Do not handle	????0.096	????0.10
Water	????0.095	????0.09
			?1.5PC-1.5G	????0.110	????0.10
?2.4PC-2.4G	????0.109	????0.10
			?3.2PC-3.2G	????0.104	????0.10
?1.5PC-2.3G	????0.110	????0.11
			?1.6PC-3.2G	????0.118	????0.11
?2.5PC-1.6G	????0.118	????0.11
			?2.4PC-3.3G	????0.108	????0.11
?3.3PC-1.6G	????0.095	????0.10
			Do not handle	????0.200	????0.11
?3.3PC-1.6G	????0.200	????0.11
			?2.4PC-3.3G	????0.220	????0.11
?1.5PC-1.5G	????0.200	????0.11

Table 9: the processing again of rehydrated paper pulp

Handle	Separate (kilowatt-hour/ton)	TENSILE STRENGTH (pound/inch)	5K density (gram/cc)
				Water	????23.9	????78.6	????0.53
?2.0PC-4.06G	????19.9	????51.4	????0.60
				?2.02PC-2.02G	????18.8	????31.3	????0.56
?2.1PC-3.17G	????18.8	????51.5	????0.58
				?3.06PC-2.04G	????13.5	????46.3	????0.56
?3.16PC-3.16G	????17.4	????33.3	????0.60
				?3.28PC-4.37G	????17.3	????38.2	????0.64
?4.11PC-2.05G	????16.2	????37.0	????0.57
				?4.2PC-3.16G	????16.6	????53.8	????0.61
?4.57PC-4.57G	????15.1	????32.6	????0.62

Table 10: the independent additive on the rehydrated paper pulp

Handle	Separate (kilowatt-hour/ton)	??DE(％)	TENSILE STRENGTH (pound/inch)	5K density (gram/cc)
					Water	????18.8	????85	????74.7	????0.48
?2.0PC	????12.5	????91	????48.6	????0.52
					?3.0PC	????10.8	????89	????52.7	????0.50
?4.0PC	????16.4	????92	????48.4	????0.55
					?5.0PC	????11.5	????89	????47.6	????0.51
?2.0G	????12.0	????88	????56.5	????0.55
					?3.0G	????23.1	????91	????50.5	????0.59
?4.0G	????19.7	????81	????61.0	????0.57
					?5.0G	????19.0	????85	????59.8	????0.61

Do not interact to having between the statistical results show detackifier of two contrived experiments (table 8 and 9) and plasticizer.Handle of the wicking rate not influence of rehydrated cellulose pulp with propylene carbonate and glycerine to the densification air forming fur felt that contains 0.9% saline solution.The Kamas separation energy and the TENSILE STRENGTH of thin slice reduce with the raising of propylene carbonate content usually, yet it is interrelated to stand behind 5000 pounds of pressure the density and the amounts of glycerol in the treatment fluid of gained.In table 10, use the propylene carbonate processing just can reduce separation energy separately and also can improve into the fur rate with TENSILE STRENGTH.Separately use the glycerine in fact to have improved the separation energy of three samples in four samples and only improved the one-tenth fur rate of two samples in four samples.

Embodiment 11-handles never the cellulose pulp through super-dry

If soften processing in producing the paper pulp mill of comminution pulp thin slice, the thin slice that so just can be chosen in firm formation enters the preceding treatment fluid of using of drying stage.In the laboratory,, this process is simulated by in water, disperseing never also to use laboratory thin slice make-up machine moulding paper pulp thin slice again through the paper pulp of super-dry by what the paper pulp mill obtained.After the stage of anhydrating for the first time, the thin slice of firm moulding soften processings, then will be done as usual drying and be cut into batten of this thin slice to separate.As in the past, the softening component of handling is expressed as the percetage by weight of final products.

Table 11: handle never paper pulp through super-dry

Handle PC-glycerine (weight %)	Kamas energy (kilowatt-hour/ton)	Separative efficiency (%)	5000 pounds of density (gram/cc)	TENSILE STRENGTH (pound/inch)	2 milliliters of instillation (milliliter/gram)	Absorbability (gram/gram)	Fracture energy (gram)	Vertical wicking (cel)
									???0-0	?16.8	?87	?0.50	?58.1	?2.7	?18.3	?134.3	?0.53
???3-4	?12.0	?95	?0.62	?28.1	?2.3	?16.6	?120.5	?0.57
									???3-0	?10.0	?94	?0.53	?44.8	?2.6	?16.8	?122.5	?0.52
???0-4	?9.0	?87	?0.59	?45.5	?2.0	?16.5	?129.2	?0.47

* PC is a propylene carbonate.

Never the paper pulp through super-dry was identical with once dry paper pulp excessively to the softening reactive mode of handling of the present invention.No matter propylene carbonate uses separately still and glycerine uses together, can be to the thin slice unsticking, and the separation energy that reduced has all confirmed this with the separative efficiency that has improved.Use glycerine to soften the thin slice that is used to separate effectively separately, the evidence of TENSILE STRENGTH aspect is also arranged, but it can not improve separative efficiency.

As by former embodiment desired, the easness of densification (with 450 grams/square metre the density that after 5000 pounds of pressure following moment compactings, obtains of gas felt) be the function of the glycerol plasticizer that exists in the cellulose fibre.Vertical wicking experiment shows organic detackifier of the present invention, is representative with the propylene carbonate, does not have secondary face to ring to the fluid delivery capability of the cellulosic fibrous structure of air forming.Softening processing may reduce absorbability a little, has some and reduces but can suspect, because to reach the required treated fiber of same weight less with undressed fiber.

Embodiment 12-handles the paper pulp thin slice of drying

Different final absorbent products may be benefited from densification in various degree.For converter, want to have the detailed bill that need not keep different paper pulp and the flexibility that can produce series of products, a method that can adopt is that paper pulp is carried out online improvement.This can spray a small amount of softening agent concentrate above it and finish at an easy rate by enter the hammer-mill forward direction at the paper pulp thin slice.The real advantage of this way is that softening processing can be carried out on converter equipment, rather than is confined on the pulp production plant.In following example, the amount that is added to propylene carbonate on each thin slice and glycerine is constant respectively to be controlled at 3 and 4%.The total amount of the water in the thin slice is transferred to 20% with 2% increment by 12%.

Table 12: handle the dry pulp thin slice

Handle	Moisture %	Separation energy (kilowatt-hour/ton)	Separative efficiency (%)	TENSILE STRENGTH (pound/inch)	5K density (gram/cc)
						Do not handle	????6.3	????25.8	????89	????101.0	????0.51
Do not handle	????12	????20.6	????78	????102.0	????0.52
						Do not handle	????14	????18.8	????78	????87.6	????0.46
Do not handle	????16	????18.5	????74	????85.5	????0.44
						Do not handle	????18	????21	????77	????95.3	????0.42
Do not handle	????20	????16.8	????79	????98.3	????0.46
?3PC-4G	????12	????19	????90	????65.9	????0.57
						?3PC-4G	????14	????16.4	????93	????71.1	????0.59
?3PC-4G	????16	????15.5	????91	????51.1	????0.56
						?3PC-4G	????18	????18.5	????89	????60.7	????0.59
?3PC-4G	????20	????18.1	????87	????55.5	????0.59

Water spray can reduce separation energy significantly under the situation of sacrificial separation efficient simply on hammer-mill forward direction paper pulp thin slice.The mixture of propylene carbonate and glycerine also can reduce separation energy but have the advantage that additional not damaging separates (becoming hair) efficient.Only through the TENSILE STRENGTH of the thin slice of water treatment than those through detackifier and plasticizer handle high a lot.450 gram/square metre gas felt pans so that same pressure compacting is made for the fur paper pulp of being handled by propylene carbonate and glycerine can obtain higher density.

Claims (21)

1. the method for the plain paper pulp of softening fibre comprises contacting with paper pulp with aqueous solution of plasticizer containing detackifier.

2. according to the process of claim 1 wherein that detackifier is selected from the low alkyl group acid esters of polyol, the cyclic ester of polyol, alkyl ether, and aryl oxide, and wherein the amount of detackifier is about 0.1 to 50 weight % of cellulose fibre.

3. spray containing the detackifier of 2 to 75 weight % and the aqueous solution of plasticizer of 2 to 75 weight % according to the process of claim 1 wherein that contact procedure comprises.

4. according to the method for claim 1, wherein plasticizer is selected from low-grade alkylamine, low alkyl group, low alkyl group, diamines, urea replaces urea, glycerine, list and two-sugar, molecular weight is lower than 1200 polyethylene glycol, and molecular weight is lower than 1000 polypropylene glycol, and wherein plasticizer is about 0.1 to 20% of cellulose fibre weight.

5. according to the process of claim 1 wherein that detackifier is selected from propylene carbonate, ethylene carbonate, glycerol triacetate, ethylene acetate, diethylene glycol diacetate, propylene-glycol diacetate, and carbonic acid hydroxyl methylvinyl ester.

6. according to the process of claim 1 wherein that plasticizer is selected from glycerine, glucose, and polyethylene glycol oxide.

7. according to the process of claim 1 wherein that detackifier comprises that propylene carbonate and plasticizer comprise glycerine.

8. according to the process of claim 1 wherein that detackifier comprises that glycerol triacetate and plasticizer comprise glycerine.

9. according to the process of claim 1 wherein that detackifier comprises that propylene carbonate and plasticizer comprise glucose.

10. the softening pulp of producing according to the process of claim 1.

11. contain the absorbent products of the softening pulp that the method for with good grounds claim 1 produces.

12. contain the absorbent products of the softening pulp that the method for with good grounds claim 6 produces.

13. the method for the plain paper pulp of softening fibre comprises the step that paper pulp is contacted with propylene carbonate.

14. the softening pulp of producing according to the method for claim 13.

15. contain the absorbent products of the softening pulp of producing by the method for right 13.

16. a cellulose paper pulp mixture comprises: cellulose pulp; The detackifier of 3-7 weight %; And the plasticizer of 3-7 weight %.

17. the cellulose paper pulp mixture of claim 16, wherein the separative efficiency of cellulose pulp be at least about 96% and Kamas mill can be about 22.9 kilowatt-hours/ton or lower.

18. the cellulose paper pulp mixture of claim 16, wherein cellulose pulp; Detackifier; And plasticizer is all in the aqueous solution.

19. the cellulose paper pulp mixture of claim 16, wherein detackifier comprises that propylene carbonate and plasticizer comprise glucose.

20. the cellulose paper pulp mixture of claim 16, wherein detackifier comprises that propylene carbonate and plasticizer comprise glycerine.

21. the cellulose paper pulp mixture of claim 16, wherein detackifier comprises that glycerol triacetate and plasticizer comprise glycerine.

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