CN106633036B - Reaction kettle is used in a kind of halogen-free flame-proof antistatic nylon 6 and preparation method thereof and preparation - Google Patents
Reaction kettle is used in a kind of halogen-free flame-proof antistatic nylon 6 and preparation method thereof and preparation Download PDFInfo
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- CN106633036B CN106633036B CN201611020735.6A CN201611020735A CN106633036B CN 106633036 B CN106633036 B CN 106633036B CN 201611020735 A CN201611020735 A CN 201611020735A CN 106633036 B CN106633036 B CN 106633036B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
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- Organic Chemistry (AREA)
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Abstract
The present invention provides a kind of halogen-free flame-proof antistatic nylon 6, preparation method and preparation reaction kettle, the components by weight percent of halogen-free flame-proof antistatic nylon 6 slice are as follows: 15-18 parts of organic phosphorus flame retardant；1-2 parts of composite antistatic agent；3-5 parts of fire retarding synergist；80-95 parts of hexyl propionamide；0.05-10 parts of stabilizer.Pass through flanged joint between reaction kettle ontology top half and stirring area；The side wall of stirring area is equipped with form；Control device is set to the exterior side wall of reaction kettle ontology；Agitating device is set to the stirring area of reaction kettle body interior；Agitating device includes retarder, shaft a and stirring wheel；Retarder is set to reaction kettle body exterior any position；Shaft a connects retarder；The shaft a is located at the hemispheric planar section in reaction kettle lower half portion, and by the centre of sphere, the present invention improves the flame retardant property and antistatic property of nylon 6 slice simultaneously, and the two performance reaches corresponding balance, increases the mixing area of reaction kettle.
Description
Technical field
The present invention relates to textile technology field more particularly to a kind of halogen-free flame-proof antistatic nylon 6, preparation method and preparation
Use reaction kettle.
Background technique
Nylon 6 fiber has a series of excellent performances, but there is also disadvantage, as modulus is low, fast light resistance to heat differential, it is easy to aging,
Antistatic property difference etc..With the improvement of living standards, people have not exclusively been satisfied with traditional fibre bring warming effect, more
Add pursuit functionalization, fining, health, quality.Compared with developed countries, China has independent intellectual property right at present
Nylon fiber new product it is considerably less, really for industrialization kind it is then less, secondly nylon fiber price compared with polyester fiber
Height, fiber series of products must be located at high-end level, just can guarantee the competitiveness of enterprise.Nylon 6 is translucent or opaque
Milky half hitch crystalline form polymer, its feature are that thermodynamic property is excellent, and lightweight, good toughness, chemicals-resistant and durability are good,
Also there is good wearability, self-lubrication.Current pure 6 fire proofing flame retardant property of nylon can only accomplish 1.6mm batten
UL94V-0 grade, simultaneously.But polyamide fibre macromolecular is more sensitive to light and heat, and fast light and heat-resistant stability is poor, in the application easy xanthochromia
Embrittlement, dyeing and printing fabric fugitive color are strongly declined to a great extent long afterwards using day, therefore it is necessary to are carried out to nylon fibre ultraviolet
Line protective finish.And needing to use reaction unit in 6 preparation process of nylon, reaction unit in the prior art stirs not because of it
Sufficiently, so that disperse between molecule it is insufficient, the specific surface area of contact it is small, can not optimize, maximumlly function grain
The effect of son, the automation ingredient of simultaneous reactions kettle be not high.
Existing pertinent literature improves nylon 6 fiber at present, such as Chinese patent CN103421184A is disclosed
A kind of preparation method of chinlon 6 section is dissolved into liquid including step 1, by the caprolactam of 90~100 parts by weight, is added 0.5
The ultraviolet absorbing agent of the initiator of~3 parts by weight and 0.1~1.0 parts by weight, is mixed evenly；Step 2 will stir evenly
Liquid afterwards is added in reaction kettle, and nitrogen charging displaced air is heated slowly to 220~260 DEG C, with stirring for 100~120r/min
5~10h of speed responsing is mixed, discharge is simultaneously sliced after sink is cooling, is sliced after being polymerize；Step 3 will be sliced after polymerization with 80
~100 DEG C water hot extraction 30 hours, 50 DEG C of air blow drying surface moistures are sliced after must extracting；Step 4 will be sliced use after extraction
Vacuum oven obtains chinlon 6 section in 100~120 DEG C of dry 7~9h.Although being added to corresponding ultraviolet light in the invention to inhale
Agent is received, improves the intensity of nylon 6 fiber accordingly, but do not coordinate flame retardant property and antistatic property from the invention, this
The invention of sample can only meet the needs of one side.Chinese patent CN105195071A discloses a kind of efficient hybrid reactor, packet
Reaction kettle body is included, feed inlet, discharge port, blender, air hose, air blower, the feed inlet setting is at the top of reaction kettle body, institute
Discharge port setting is stated in reaction kettle body bottom, the air hose enters in reaction kettle one through to bottom at the top of reaction kettle body,
The air blower connects outside reaction kettle body with air hose.The mixing area of reactor agitator in the invention is small, can not
Realize that reactant is sufficiently mixed, especially in the case where reactant capacity is excessive or too small.
Summary of the invention
For overcome it is existing in the prior art can not achieve reactant be sufficiently mixed, the mixing area of reactor agitator it is small
The problems such as, the present invention provides a kind of halogen-free flame-proof antistatic nylon 6, preparation method and preparation reaction kettles.
The present invention provides a kind of components by weight percent of halogen-free flame-proof antistatic nylon 6 slice are as follows:
The organic phosphorus flame retardant is one or more of phosphite ester, organophosphorated salt and polymeric phosphoric acid ester；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=1
~1.5:2~3.
The stabilizer is the one or more of hindered amine stabilizer and hypophosphites stabilizer.
The present invention also provides a kind of halogen-free flame-proof antistatic nylon 6 slice preparation methods: steps are as follows:
Step 010, hexyl propionamide the pretreatment of hexyl propionamide: is subjected to vacuum drying 1-3h, vacuum degree 0.05-
10kpa；
Step 020, stabilizer is added in hexyl propionamide after the pre-treatment, is mixed evenly to obtain mixture a；It is described
Mixture a placement is slowly heated to 200-230 DEG C in a kettle, and heating time 3-5h obtains mixture b；
Step 030, halogen-free flame retardants, fire retarding synergist and composite anti-static are sequentially added in the mixture b, in 100-
It is mixed at 120 DEG C, mixing speed 100-120r/min, mixing time 5-8h obtains mixture c；
Step 040, mixture c is subjected to melt spinning.
Further, the components by weight percent of the halogen-free flame-proof antistatic nylon 6 slice are as follows:
The organic phosphorus flame retardant is in phosphite ester, organophosphorated salt and polymeric phosphoric acid ester；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=
1.3:2.5。
The stabilizer is hindered amine stabilizer and hypophosphites stabilizer.
Further, the halogen-free flame-proof antistatic nylon 6 slice preparation method: steps are as follows:
Step 010, it pre-processes hexyl propionamide: hexyl propionamide is subjected to vacuum drying 2h, vacuum degree 6kpa；
Step 020, stabilizer is added in hexyl propionamide after the pre-treatment, is mixed evenly to obtain mixture a；It is described
Mixture a placement is slowly heated to 220 DEG C in a kettle, and heating time 4h obtains mixture b, is cooled to room temperature；
Step 030, halogen-free flame retardants, fire retarding synergist and composite anti-static are sequentially added in the mixture b, 110
It is mixed at DEG C, mixing speed 120r/min, mixing time 7h obtains mixture c；
Step 040, mixture c is subjected to melt spinning.
The present invention also provides a kind of reaction kettles for halogen-free flame-proof antistatic nylon 6 slice preparation；
The reaction kettle includes reaction kettle ontology, control device, agitating device, vacuum plant and microwave heating equipment；Institute
Reaction kettle ontology top half is stated equipped with microwave heating equipment, the vacuum plant is close to microwave heating equipment；The reaction kettle
Ontology lower half portion is stirring area, and shape is sphere, and innovative point is: the reaction kettle ontology top half and lower half portion
Between pass through flanged joint；The side wall of the stirring area is additionally provided with form；The control device is set to the outside of reaction kettle ontology
Side wall；Agitating device is set to the stirring area of reaction kettle body interior；The agitating device includes retarder, shaft a and stirring wheel；
The retarder is set to reaction kettle body exterior any position；The shaft a connection retarder；The shaft a is located at described anti-
The hemispheric planar section in kettle lower half portion is answered, and passes through the centre of sphere.
Further, the microwave heating equipment includes microwave operational chamber and microwave generator, and the microwave operational chamber is set
In the entire inner wall of reaction kettle ontology；The microwave operational chamber is equipped with interlayer, and the interlayer is divided into first layer stainless-steel sheet, the
Two layers are micro-wave screening net and third layer is stainless-steel sheet.
Further, the stirring wheel is rearranged by multiple impellers, and the impeller is detachable impeller；The impeller
Inner diametric step is equipped with threaded hole a.The agitating device can change the number of impeller according to the working condition actually stirred, so that
Reaction kettle can satisfy the use under different working conditions.
Further, the impeller diameter gradual change trend of the arrangement be from left to right or be from right to left first to become larger to become again
Small, the impeller diameter at the position of stirring wheel middle is maximum value, and the trend of diameter variation is with the reaction kettle sheet
Diametrically variation tendency is consistent in the section of body lower half portion sphere.The agitating device of reaction kettle increases stirring in the present invention
Area, so that mixture obtains full and uniform stirring.
Further, the surface the shaft a is equipped with keyway；The keyway along shaft a ring-shaped section and ring-shaped array distribution, and
Be equally spaced multiple keyways on the axial direction of shaft a.
Further, rotating plate is equipped in the keyway, the rotating plate middle is equipped with through-hole, when the keyway is not used,
Rotating plate is in buckling state；When the rotating plate is buckling state, screw thread is equipped at the relative position of the shaft a and rotating plate through-hole
Hole b is fixed rotating plate and shaft a using bolt.
Compared with prior art, the beneficial effects of the present invention are:
(1) change of halogen-free flame-proof antistatic nylon 6 slice ingredient and preparation method of the invention can improve simultaneously
The flame retardant property and antistatic property of nylon 6 slice, the two performance reach corresponding balance；Flame retardant property reaches UL94V-0 etc.
Grade, while resistivity is down to 8.2 × 107Ω。
(2) flame retardant performance can be improved in fire retarding synergist of the invention, while can reduce cost again；It is added compound anti-
Enhancing antistatic property can be improved in electrostatic agent, avoids because single antistatic agent adjusts the limitation to resistivity effects.
(3) mixture a may make to obtain uniformly adding by microwave heating in the nylon 6 slice preparation method in the present invention
Heat, keep from heat unevenness, influences subsequent product performance.
(4) reaction kettle used in the nylon 6 slice preparation in the present invention improves the automation journey of nylon 6 slice preparation
Degree.
(5) agitating device of reaction kettle increases mixing area in the present invention, so that mixture obtains full and uniform stir
It mixes, improves stirring precision.The agitating device can change the number of impeller according to the working condition actually stirred simultaneously, so that
Reaction kettle can satisfy the use under different working conditions.
Detailed description of the invention
Fig. 1 is nylon 6 slice preparation flow figure in embodiment 1；
Fig. 2 is the side schematic view of reaction kettle；
Fig. 3 is agitating device schematic diagram；
Fig. 4 is keyway position view on shaft a；
Fig. 5 is shaft a upper rotating plate scheme of installation；
Fig. 6 is the shaft and impeller scheme of installation when keyway number is 6 on section；
Fig. 7 is the shaft and impeller scheme of installation when keyway book is 3 on section.
It marks in conjunction with attached drawing and on it:
1- reaction kettle ontology, 2- vacuum plant, 3- microwave generator, 4- microwave operational chamber, 5- agitating device, 51- impeller,
52- shaft a, 53- step, 521- keyway, 522- threaded hole b, 6- form, 71- rotating plate, 72- threaded hole a72,73- shaft b, 8-
Sunk screw.
Specific embodiment
Below in conjunction with drawings and examples, the present invention will be described in further detail.It should be appreciated that described herein
Specific examples are only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1
A kind of components by weight percent of halogen-free flame-proof antistatic nylon 6 slice are as follows:
The organic phosphorus flame retardant is phosphite ester；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=
1:2。
The stabilizer is hindered amine stabilizer.
The halogen-free flame-proof antistatic nylon 6 slice preparation method, as described in Figure 1: steps are as follows:
Step 010, it pre-processes hexyl propionamide: hexyl propionamide is subjected to vacuum drying 1h, vacuum degree 0.05kpa；
Step 020, stabilizer is added in hexyl propionamide after the pre-treatment, is mixed evenly to obtain mixture a；It is described
Mixture a placement carries out microwave heating in a kettle, and heating temperature is slowly heated to 200 DEG C, and heating time 3h is mixed
Object b is closed, is cooled to room temperature；It may make that mixture a is evenly heated by microwave heating, keep from heat unevenness, influences subsequent
Properties of product.
Step 030, halogen-free flame retardants, fire retarding synergist and composite antistatic agent are sequentially added in the mixture b,
It is mixed at 100 DEG C, mixing speed 100r/min, mixing time 5h obtains mixture c.It, can using fire retarding synergist
To improve flame retardant performance, while cost can be reduced again；Composite antistatic agent, which is added, can be improved enhancing antistatic property, avoid
Because single antistatic agent adjusts the limitation to resistivity effects.
Step 040, mixture c is subjected to melt spinning.
The present invention also provides a kind of reaction kettles for halogen-free flame-proof antistatic nylon 6 slice preparation；Such as Fig. 2 institute
Show, the reaction kettle includes reaction kettle ontology 1, control device, agitating device 5, vacuum plant 2 and microwave heating equipment；It is described
1 top half shape of reaction kettle ontology is cylinder, and the upper half is equipped with microwave heating equipment；1 lower half of reaction kettle ontology
Dividing shape is hemispherical, and lower half portion is stirring area；Pass through flange between 1 top half of reaction kettle ontology and lower half portion
Connection；The side wall of the stirring area is additionally provided with form 6, and the stirring state in stirring area can be observed through form 6, passes through stirring
The operating condition of situation adjustment agitating device 5.1 top of reaction kettle ontology is equipped with feed inlet, and lower part is equipped with discharge port；The control
Device is set to the exterior side wall of reaction kettle ontology top half, and the control device is for controlling agitating device 5, vacuum plant 2
With the work of microwave heating equipment；Agitating device 5 is set to the stirring area inside reaction kettle ontology 1；The control device is located at anti-
Heating temperature, heating time and retarder needed for answering 1 exterior side wall of kettle ontology, technical staff that can set by control device
Revolving speed.The vacuum plant 2 is set to the top of reaction kettle ontology 1 close to feed inlet.
The microwave heating equipment includes microwave operational chamber 4 and microwave generator 3, and the microwave operational chamber 4 is set to reaction
The entire inner wall of kettle ontology 1；The microwave operational chamber 4 is equipped with interlayer, and the interlayer is divided into first layer stainless-steel sheet, the second layer
It is stainless-steel sheet for micro-wave screening net and third layer, prevents microwave leakage.The micro-wave screening net uses aluminum gauze screen.Such as
Shown in Fig. 3, the agitating device 5 includes retarder, shaft a52 and stirring wheel；The retarder is set to outside reaction kettle ontology 1
Any position；The shaft a52 connection retarder；The shaft a52 is located at the hemispheric plane in reaction kettle lower half portion
Part, and pass through the centre of sphere.
The stirring wheel is rearranged by multiple impellers 51, and the impeller 51 is detachable impeller 51；The impeller 51
53 face of inner diametric step be equipped with threaded hole a72；The 51 Diameter Gradual Change trend of impeller of the arrangement is from left to right or from dextrad
A left side is first to become larger to become smaller again, and 51 diameter of impeller at the position of stirring wheel middle is maximum value, diameter variation
Diametrically variation tendency is consistent with the section of the 1 lower half portion sphere of reaction kettle ontology for trend；The agitating device 5 can
To ensure to have large-scale mixing area, so that mixture obtains full and uniform stirring, stirring precision is improved.It is described to stir
The stirring rate for mixing device 5 is controlled by control device, and the impeller 51 on the stirring wheel can carry out dismantling while of impeller 51
Number can be by carrying out appropriate adjustment according to the actual situation in actual use.
As shown in figure 4, the surface the shaft a52 is equipped with keyway 521；Ring-shaped section and ring-shaped of the keyway 521 along shaft a52
Array distribution, and multiple keyways 521 that are equally spaced on the axial direction of shaft a52；Along the section of shaft a52 in the present embodiment
521 quantity of keyway is 6, such as Fig. 6.It uses 521 minimum number of keyway to be distributed for 3, such as Fig. 7, guarantees impeller 51 in shaft a52
On stability, prevent from sliding during rotation.As shown in figure 5, rotating plate 71 is equipped in the keyway 521, described turn
71 middle of plate is equipped with through-hole, and when the keyway 521 is not used, rotating plate 71 is in buckling state；The rotating plate 71 is to fasten shape
When state, threaded hole b522 is equipped at the relative position of the shaft a52 and 71 through-hole of rotating plate, using bolt by rotating plate 71 and shaft
A52 is fixed, and shaft a52 is avoided to cause the folding of rotating plate 71 during rotation；The diameter of the through-hole and the screw thread of impeller 51
Hole a72 diameter is consistent.It is fixed using sunk screw 8 by threaded hole a72 and through-hole between the rotating plate 71 and impeller 51
Connection.The side of the rotating plate 71 is connected with 521 side wall of keyway, and connecting place uses shaft b73；On the same section shaft a52
Keyway 521 is column, and a column keyway 521 is for fixing an impeller 51；The columns of the keyway 521 is more than or equal to the number of impeller 51.
When keyway 521 is not used by, rotating plate 71 is fixed with shaft a52；When impeller 51 and fixed keyway 521, bolt is unclamped, is turned
Plate 71 is overturn along shaft b73, and 53 face of step of impeller 51 is bonded with rotating plate 71, threaded hole and the rotating plate 71 of the impeller 51
Through-hole is in same center line, is fixedly connected with the two using sunk screw 8.In the agitating device 5 impeller 51 detachably and
It is fixed, while the number of impeller 51 can be changed according to the working condition actually stirred, so that reaction kettle can satisfy different operating conditions
Under the conditions of use.
The 1 top half inner wall of reaction kettle ontology is equipped with temperature sensor；The stirring area inner wall is equipped with the sensing that tests the speed
Device；The control device includes vacuum-ness regulator, temperature control device, rotation speed regulating and controlling device, wireless device and controller；It is described
Temperature control device, rotation speed regulating and controlling device, vacuum-ness regulator and wireless device are successively connected with controller, are controlled by controller
The working condition of temperature control device, rotation speed regulating and controlling device, vacuum-ness regulator and wireless device；The vacuum-ness regulator control
Vacuum plant processed carries out vacuum degree adjusting to reaction kettle ontology 1；The temperature aperture apparatus includes temperature regulation unit and monitoring temperature
Unit, the temperature monitoring unit receives temperature sensor signal, and transmits a signal to temperature regulation unit；The temperature tune
Control unit is connect with microwave heating equipment, and temperature regulation unit controls the frequency of microwave generator 3, to control temperature rising
Rate.The rotation speed regulating and controlling device includes rotary speed controling unit and monitor speed unit；The monitor speed unit reception is tested the speed
Tach signal is transferred to rotary speed controling unit by the tach signal of sensor；The rotary speed controling unit is connected with retarder, control
The revolving speed of retarder processed controls the revolving speed of stirring wheel by retarder.The wireless device includes wireless generating device, wirelessly connects
Receiving apparatus and external display device.The external display device is at any position outside reaction kettle, external display device
In in the coverage area of wireless generating device, by wireless device by reaction kettle temperature signal and tach signal be transferred to it is outer
Portion's equipment, by remotely controlling in external display device, control signal is received by radio receiver, be transferred to controller into
Row regulation.
Working principle:
Hexyl propionamide is entered in reaction kettle by feed inlet, vacuum-ness regulator, vacuum degree are controlled by controller
Vacuum degree in reaction kettle is set as 0.05kpa by regulating device, and concurrently setting vacuum drying time is 1h, and vacuum degree is adjusted at this time
Device controls vacuum plant 2 and works；When vacuum degree reaches setting value, vacuum plant 2 stops working；It is added in a kettle at this time
Stabilizer, controller control agitating device 5 are mixed, and the revolving speed and mixing time of the agitating device 5 pass through revolving speed
Control unit setting, is stirred for uniformly obtaining mixture a；Controller starts microwave to the mixture a after mixing evenly
Device 3；It by temperature regulation unit set temperature and heating time, sets heating temperature and is slowly heated to 200 DEG C, heating time is
3h, the temperature regulation unit are connect with microwave heating equipment, and temperature regulation unit controls the frequency of microwave generator 3, thus
Control the rate that temperature rises；When temperature reaches setting value in reaction kettle, the temperature monitoring unit receives temperature sensor letter
Number, and temperature regulation unit is transmitted a signal to, temperature regulation unit is opened and closed microwave generator 3, is simultaneously stopped 5 work of agitating device
Make, obtains mixture b at this time, be cooled to room temperature；It may make that mixture a is evenly heated by microwave heating, keep from heat
Unevenness influences subsequent product performance.After obtaining mixture b, successively in a kettle be added halogen-free flame retardants, fire retarding synergist and
Flame retardant performance can be improved using fire retarding synergist in composite antistatic agent, while can reduce cost again；Be added it is compound resist it is quiet
Enhancing antistatic property can be improved in electric agent, avoids because single antistatic agent adjusts the limitation to resistivity effects.
The rotary speed controling unit is connected with retarder, controls the revolving speed of retarder, and the rotary speed controling unit setting is stirred
Mix that speed is 100r/min and mixing time is 5h, while temperature regulation unit set temperature heating temperature is to mix at 100 DEG C
Stirring, while tach signal is measured by velocity sensor in whipping process, tach signal is transferred to rotary speed controling unit,
Obtain mixture c.Mixture c is placed in fusion apparatus and melts from the discharge port outflow in reaction kettle by the mixture c
Melt spinning.Impeller 51 on the agitating device 5 can be dismantled, while the number of impeller 51 can be by root in actual use
Appropriate adjustment is carried out according to actual conditions.When the keyway 521 on the surface the shaft a52 is not used, rotating plate 71 is in buckling state；Institute
When to state rotating plate 71 be buckling state, it is equipped with threaded hole b522 at the relative position of the shaft a52 and 71 through-hole of rotating plate, using spiral shell
Bolt fixes rotating plate 71 and shaft a52, and shaft a52 is avoided to cause the folding of rotating plate 71 during rotation；The rotating plate 71 with
It is fixedly connected using sunk screw 8 by threaded hole a72 and through-hole between impeller 51.Key on the same section shaft a52
Slot 521 is column, and a column keyway 521 is for fixing an impeller 51；The columns of the keyway 521 is more than or equal to the number of impeller 51.When
When keyway 521 is not used by, rotating plate 71 is fixed with shaft a52；When impeller 51 and fixed keyway 521, bolt is unclamped, rotating plate
71 overturn along shaft b73, and 53 face of step of impeller 51 is bonded with rotating plate 71, the threaded hole of the impeller 51 and leading to for rotating plate 71
Hole is in same center line, is fixedly connected with the two using sunk screw 8.The wireless device includes wireless generating device, nothing
Line reception device and external display device.The external display device is set to any position outside reaction kettle, and external display is set
In the standby coverage area in wireless generating device, by wireless device by reaction kettle temperature signal and tach signal transmit
To external equipment, by remotely controlling in external display device, control signal is received by radio receiver, is transferred to control
Device is regulated and controled.
Embodiment 2
The present embodiment is different from the first embodiment in: the organic phosphorus flame retardant is phosphite ester and organic phosphorus
Salt；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=
1:3。
The stabilizer is hypophosphites stabilizer.
Embodiment 3
The present embodiment and the first and second embodiment the difference is that: the organic phosphorus flame retardant is phosphite ester, organic
Microcosmic salt and polymeric phosphoric acid ester；
The composite antistatic agent is antistatic agent: polyether ester amides and polyethylene oxide；The polyether ester amides: polycyclic
Oxidative ethane=1.5:2.
The stabilizer is hindered amine stabilizer and hypophosphites stabilizer.
Embodiment 4
The present embodiment is different from the third embodiment place and is: the composite antistatic agent is antistatic agent: polyether ester acyl
Amine and polyethylene oxide；The polyether ester amides: polyethylene oxide=1.5:3.
Embodiment 5
The present invention provides a kind of components by weight percent of halogen-free flame-proof antistatic nylon 6 slice are as follows:
The organic phosphorus flame retardant is phosphite ester；
The composite antistatic agent is antistatic agent: polyether ester amides and polyethylene oxide；The polyether ester amides: polycyclic
Oxidative ethane=1:2.
The stabilizer is hindered amine stabilizer.
The halogen-free flame-proof antistatic nylon 6 slice preparation method: steps are as follows:
Step 010, it pre-processes hexyl propionamide: hexyl propionamide is subjected to vacuum drying 1.5h, vacuum degree 2kpa；
Step 020, stabilizer is added in hexyl propionamide after the pre-treatment, is mixed evenly to obtain mixture a；It is described
Mixture a placement is slowly heated to 210 DEG C in a kettle, and heating time 3.5h obtains mixture b, is cooled to room temperature；
Step 030, halogen-free flame retardants, fire retarding synergist and composite anti-static are sequentially added in the mixture b, 105
It is mixed at DEG C, mixing speed 105r/min, mixing time 6h obtains mixture c；
Step 040, mixture c is subjected to melt spinning.
Embodiment 6
The present embodiment and the 5th embodiment the difference is that: the organic phosphorus flame retardant is phosphite ester and organic phosphorus
Salt；
The composite antistatic agent is antistatic agent: polyether ester amides and polyethylene oxide；The polyether ester amides: polycyclic
Oxidative ethane=1:3.
The stabilizer is hypophosphites stabilizer.
Embodiment 7
The present embodiment and the five, the six embodiments the difference is that: the organic phosphorus flame retardant is phosphite ester, organic
Microcosmic salt and polymeric phosphoric acid ester；
The composite antistatic agent is antistatic agent: polyether ester amides and polyethylene oxide；The polyether ester amides: polycyclic
Oxidative ethane=1.5:2.
The stabilizer is hindered amine stabilizer and hypophosphites stabilizer.
Embodiment 8
The present embodiment and the 7th embodiment the difference is that: the composite antistatic agent be antistatic agent: polyether ester acyl
Amine and polyethylene oxide；The polyether ester amides: polyethylene oxide=1.5:3.
Embodiment 9
The present invention provides a kind of components by weight percent of halogen-free flame-proof antistatic nylon 6 slice are as follows:
The organic phosphorus flame retardant is phosphite ester；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=
1:2。
The stabilizer is hindered amine stabilizer.
The halogen-free flame-proof antistatic nylon 6 slice preparation method: steps are as follows:
Step 010, it pre-processes hexyl propionamide: hexyl propionamide is subjected to vacuum drying 3h, vacuum degree 10kpa；
Step 020, stabilizer is added in hexyl propionamide after the pre-treatment, is mixed evenly to obtain mixture a；It is described
Mixture a placement is slowly heated to 230 DEG C in a kettle, and heating time 5h obtains mixture b, is cooled to room temperature；
Step 030, halogen-free flame retardants, fire retarding synergist and composite anti-static are sequentially added in the mixture b, 120
It is mixed at DEG C, mixing speed 120r/min, mixing time 8h obtains mixture c；
Step 040, mixture c is subjected to melt spinning.
Embodiment 10
The present embodiment and the 9th embodiment the difference is that: the organic phosphorus flame retardant is phosphite ester and organic phosphorus
Salt；
The composite antistatic agent is antistatic agent: polyether ester amides and polyethylene oxide；The polyether ester amides: polycyclic
Oxidative ethane=1:3.
The stabilizer is hypophosphites stabilizer.
Embodiment 11
The present embodiment and the nine, the ten embodiments the difference is that: the organic phosphorus flame retardant is phosphite ester, organic
Microcosmic salt and polymeric phosphoric acid ester；
The composite antistatic agent is antistatic agent: polyether ester amides and polyethylene oxide；The polyether ester amides: polycyclic
Oxidative ethane=1.5:2.
The stabilizer is hindered amine stabilizer and hypophosphites stabilizer.
Embodiment 12
The present embodiment and the 11st embodiment the difference is that: the composite antistatic agent be antistatic agent: polyether ester
Amide and polyethylene oxide；The polyether ester amides: polyethylene oxide=1.5:3.
Embodiment 13
The components by weight percent of the halogen-free flame-proof antistatic nylon 6 slice are as follows:
The organic phosphorus flame retardant is in phosphite ester, organophosphorated salt and polymeric phosphoric acid ester；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=
1.5:2。
The stabilizer is hindered amine stabilizer and hypophosphites stabilizer.
The halogen-free flame-proof antistatic nylon 6 slice preparation method: steps are as follows:
Step 010, it pre-processes hexyl propionamide: hexyl propionamide is subjected to vacuum drying 2h, vacuum degree 6kpa；
Step 020, stabilizer is added in hexyl propionamide after the pre-treatment, is mixed evenly to obtain mixture a；It is described
Mixture a placement is slowly heated to 220 DEG C in a kettle, and heating time 4h obtains mixture b, is cooled to room temperature；
Step 030, halogen-free flame retardants, fire retarding synergist and composite anti-static are sequentially added in the mixture b, 110
It is mixed at DEG C, mixing speed 120r/min, mixing time 7h obtains mixture c；
Step 040, mixture c is subjected to melt spinning.
6 spinning of nylon obtained in embodiment 1-13 is placed under simply supported beam notch impact strength testing machine and measures notch
Impact strength is placed under tensile strength test instrument and measures tensile strength and elongation at break, and is sentenced using vertical burn method
Disconnected flame retardant property, measures the resistivity of 6 spinning of nylon, and gained performance parameter is in table 1.
Table 1 is that the manufactured of embodiment 1-13 meets material property table
It can be seen that from the performance table of embodiment 1-13 in the constituent ratio of embodiment 13 and the change of technological parameter
The flame retardant property and resistivity of nylon 6 slice are enhanced, while when the polyether ester acyl in embodiment 3,7 and embodiment 11
Amine: when the ratio of polyethylene oxide is in 1.5:2, vertical combustion performance is significantly improved, therefore described in the present invention
Polyether ester amides: the ratio of polyethylene oxide is optimal should to use 1.5:2.Halogen-free flame-proof antistatic nylon 6 slice of the invention at
The flame retardant property and antistatic property for dividing the change with preparation method that can improve nylon 6 slice simultaneously, the two performance reach
Corresponding balance；Flame retardant property reaches UL94V-0 grade, while resistivity is down to 8.2 × 107Ω。
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification and
Environment, and can be changed within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge
It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention
In scope of protection of the claims.
Claims (8)
1. a kind of preparation method of halogen-free flame-proof antistatic nylon 6 slice, it is characterised in that:
The components by weight percent of the halogen-free flame-proof antistatic nylon 6 slice are as follows:
15-18 parts of organic phosphorus flame retardant
1-2 parts of composite antistatic agent
3-5 parts of fire retarding synergist
80-95 parts of caprolactam
0.05-10 parts of stabilizer；
The organic phosphorus flame retardant is one or more of phosphite ester, organophosphorated salt and polymeric phosphoric acid ester；
The composite antistatic agent is polyether ester amides and polyethylene oxide；The polyether ester amides: polyethylene oxide=1 ~ 1.5:
2~3；
The stabilizer is the one or more of hindered amine stabilizer and hypophosphites stabilizer；
Steps are as follows for the halogen-free flame-proof antistatic nylon 6 slice preparation method:
Step 010, caprolactam the pretreatment of caprolactam: is subjected to vacuum drying 1-3h, vacuum degree 0.05-10kPa；
Step 020, stabilizer is added in caprolactam after the pre-treatment, is mixed evenly to obtain mixture a；The mixing
Object a placement is slowly heated to 200-230 DEG C in a kettle, and heating time 3-5h obtains mixture b；
Step 030, organic phosphorus flame retardant, fire retarding synergist and composite antistatic agent are sequentially added in the mixture b,
It is mixed at 100-120 DEG C, mixing speed 100-120r/min, mixing time 5-8h obtains mixture c；
Step 040, mixture c melting extrusion is obtained into halogen-free flame-proof antistatic nylon 6 slice.
2. nylon 6 slice preparation method according to claim 1, it is characterised in that:
The halogen-free flame-proof antistatic nylon 6 slice preparation method: steps are as follows:
Step 010, it pre-processes caprolactam: caprolactam is subjected to vacuum drying 2h, vacuum degree 6kPa；
Step 020, stabilizer is added in caprolactam after the pre-treatment, is mixed evenly to obtain mixture a；The mixing
Object a placement is slowly heated to 220 DEG C in a kettle, and heating time 4h obtains mixture b, is cooled to room temperature；
Step 030, organic phosphorus flame retardant, fire retarding synergist and composite antistatic agent are sequentially added in the mixture b,
It is mixed at 110 DEG C, mixing speed 120r/min, mixing time 7h obtains mixture c；
Step 040, mixture c is subjected to melt spinning.
3. a kind of reaction kettle in halogen-free flame-proof antistatic nylon 6 slice preparation method described in claim 1, the reaction
Kettle includes reaction kettle ontology (1), control device, agitating device (5), vacuum plant (2) and microwave heating equipment；The reaction kettle
Ontology (1) top half is equipped with microwave heating equipment, and the vacuum plant (2) is close to microwave heating equipment；The reaction kettle sheet
Body (1) lower half portion is stirring area, and shape is hemisphere, it is characterised in that: reaction kettle ontology (1) top half and lower half
Pass through flanged joint between part；The side wall of the stirring area is additionally provided with form (6)；The control device is set to reaction kettle ontology
(1) exterior side wall；Agitating device (5) is set to reaction kettle ontology (1) internal stirring area；The agitating device (5) includes subtracting
Fast device, shaft a(52) and stirring wheel；The retarder is set to reaction kettle ontology (1) external any position；The shaft a(52)
Connect retarder；The shaft a(52) it is located at the hemispheroidal planar section in reaction kettle lower half portion, and pass through the centre of sphere.
4. reaction kettle according to claim 3, it is characterised in that: the microwave heating equipment includes microwave operational chamber (4)
With microwave generator (3), the microwave operational chamber (4) is set to the entire inner wall of reaction kettle ontology (1)；The microwave operational chamber
(4) it is equipped with interlayer, the interlayer is divided into first layer stainless-steel sheet, the second layer is micro-wave screening net and third layer is stainless steel steel
Plate.
5. reaction kettle according to claim 3, it is characterised in that: the stirring wheel is rearranged by multiple impellers (51),
The impeller (51) is detachable impeller；The step (53) of impeller (51) internal diameter is equipped with threaded hole a(72).
6. reaction kettle according to claim 5, it is characterised in that: the diameter of the impeller (51) arranged on the stirring wheel is gradually
For change trend to be from left to right first to become larger to become smaller again, impeller (51) diameter at the position of stirring wheel middle is maximum value,
The trend of diameter variation with reaction kettle ontology (1) lower half portion sphere section diametrically variation tendency one
It causes.
7. reaction kettle according to claim 3, it is characterised in that: the shaft a(52) surface be equipped with keyway (521)；Institute
Keyway (521) is stated to be equally spaced along the ring-shaped section and ring-shaped array distribution of shaft a(52), and on the axial direction of shaft a(52)
Multiple keyways (521).
8. reaction kettle according to claim 7, it is characterised in that: rotating plate (71) are equipped in the keyway (521), described turn
Plate (71) middle is equipped with through-hole, and the keyway (521) is not used, and rotating plate (71) is in buckling state；The rotating plate (71) is
Buckling state, the shaft a(52) with threaded hole b(522 is equipped at the relative position of rotating plate (71) through-hole), will be turned using bolt
Plate (71) and shaft a(52) it is fixed.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611020735.6A CN106633036B (en) | 2016-11-21 | 2016-11-21 | Reaction kettle is used in a kind of halogen-free flame-proof antistatic nylon 6 and preparation method thereof and preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611020735.6A CN106633036B (en) | 2016-11-21 | 2016-11-21 | Reaction kettle is used in a kind of halogen-free flame-proof antistatic nylon 6 and preparation method thereof and preparation |
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| CN106633036A CN106633036A (en) | 2017-05-10 |
| CN106633036B true CN106633036B (en) | 2019-02-12 |
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| CN114957987A (en) * | 2022-07-04 | 2022-08-30 | 华润化学材料科技股份有限公司 | Flame-retardant antistatic master batch and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417715A (en) * | 2011-11-23 | 2012-04-18 | 上海日之升新技术发展有限公司 | Permanent antistatic PA6 (Polyamide 6) composite material and preparation method thereof |
| CN103819666A (en) * | 2014-02-20 | 2014-05-28 | 株洲时代新材料科技股份有限公司 | High flame retardant nylon resin and its preparation method |
| CN204074083U (en) * | 2014-10-05 | 2015-01-07 | 刘方旭 | A kind of Intelligent Single-Chip Based controls heating using microwave liquid material stirred tank |
| CN104558587A (en) * | 2015-01-30 | 2015-04-29 | 江苏弘盛新材料股份有限公司 | Photo-thermal stable nylon 6 and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130324663A1 (en) * | 2012-06-05 | 2013-12-05 | Advanced Nylons PTY. LTD. | Nylon Compositions for Forming Cast Nylon and Cast Nylon Parts |
-
2016
- 2016-11-21 CN CN201611020735.6A patent/CN106633036B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417715A (en) * | 2011-11-23 | 2012-04-18 | 上海日之升新技术发展有限公司 | Permanent antistatic PA6 (Polyamide 6) composite material and preparation method thereof |
| CN103819666A (en) * | 2014-02-20 | 2014-05-28 | 株洲时代新材料科技股份有限公司 | High flame retardant nylon resin and its preparation method |
| CN204074083U (en) * | 2014-10-05 | 2015-01-07 | 刘方旭 | A kind of Intelligent Single-Chip Based controls heating using microwave liquid material stirred tank |
| CN104558587A (en) * | 2015-01-30 | 2015-04-29 | 江苏弘盛新材料股份有限公司 | Photo-thermal stable nylon 6 and preparation method thereof |
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