CN105386151A - Polyformaldehyde fiber preparation method - Google Patents

Polyformaldehyde fiber preparation method Download PDF

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Publication number
CN105386151A
CN105386151A CN201510955587.6A CN201510955587A CN105386151A CN 105386151 A CN105386151 A CN 105386151A CN 201510955587 A CN201510955587 A CN 201510955587A CN 105386151 A CN105386151 A CN 105386151A
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China
Prior art keywords
lubricant
polyformaldehyde
spinning
preparation
molecular weight
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CN201510955587.6A
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Chinese (zh)
Inventor
黎泽东
唐晓东
张海涛
雷琴
杨宗海
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Yunnan Yuntianhua Co Ltd
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Yunnan Yuntianhua Co Ltd
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Priority to CN201510955587.6A priority Critical patent/CN105386151A/en
Publication of CN105386151A publication Critical patent/CN105386151A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/94Monocomponent 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 other polycondensation products

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

The present invention provides a polyformaldehyde fiber preparation method which is as follows: polyformaldehyde resin is mixed with an internal lubricant, and polyformaldehyde fiber can be obtained by extrusion, pelletizing, drying and spinning, and the internal lubricant is selected from one or more internal lubricants of fatty acid ester internal lubricants, fatty alcohol internal lubricants, fatty acid amide internal lubricants and low molecular weight hydrocarbon internal lubricants. The polyformaldehyde fiber preparation method does not affect an original polyformaldehyde production line and product, has no special equipment and technology requirement, and is high in universality; at the same time by adding of the internal lubricant, the resin matrix fluidity is improved, and the polyformaldehyde fiber with excellent spinnability and high strength can be prepared.

Description

A kind of preparation method of polyformaldehyde fibre
Technical field
The present invention relates to technical field of polyformaldehyde, particularly relate to a kind of preparation method of polyformaldehyde fibre.
Background technology
Polyformaldehyde is a kind of engineering plastics of excellent combination property, as the rigidity of excellence, intensity, creep recovery performance, alkaline-resisting, solvent resistance, electrology characteristic etc., and crystallization rate is fast, be applicable to very much extruding, the conventional machining material such as injection mo(u)lding, be widely used in automobile, electric, the industry such as household electrical appliance, precision optical machinery and construction material.
Because polyformaldehyde has excellent combination property, therefore the polyformaldehyde fibre prepared by fibre-grade polyformaldehyde also inherits its most advantage, makes polyformaldehyde fibre have Gao Gang, high-strength, fiber size good stability, the advantages such as chemical resistance, especially alkali resistance are excellent.Therefore polyformaldehyde fibre is widely used in the fields such as concrete reinforced material, meshed filter material and rope.
It is necessary that spinning material possesses high molecular, but incidental be that mobility declines, there is larger impact to fiberizing and after-drawing in this; The crystalline rate of acetal resin is fast, and in the melt spinning, drawing and setting operation of fiber, fibrillation easily ruptures, and the production efficiency of polyformaldehyde fibre is low, and its suitability for industrialized production is restricted; Meanwhile, because stretching ratio is too low, fibre strength is not high, and market development and the utilization of fibre are restricted.
There is the spinnability being improved fibre by the crystallization of molecular structure adjustment resin body in prior art, thus improve the method for intensity; Also there is the mobility by improving spinning poly formaldehyde, optimizing melt-spinning technology, improve spinning efficiency, make the method that spinning is stable.Such as: patent document JP2000336098, CN1504508A, CN100334271C disclose by regulating the ratio of oxyalkylene units, crystallization control, in the hope of the obtained method of polyformaldehyde fibre with high strength, elastic modulus.But the mobility in later stage spinning process, dispersiveness are bad, affect final products performance, easily produce stress concentration point in the fibre, and fibrous fracture is frequent, and as-spun fibre stretches and is restricted, and production efficiency is low; Simultaneously, the special crystallization inhibitor of polyformaldehyde seek relative difficult, existing auxiliary agent can not realize its function, based on the rigors of technology, equipment, this complex process, cost is high, and in suitability for industrialized production enforcement, to having high input of raw material and equipment, the practicality of the polyformaldehyde fibre produced and its popularization are restricted.
Publication number is that CN102677217A Chinese patent discloses a kind of modification POM fiber and preparation method thereof, and it mixes with polyformaldehyde after nono calcium carbonate modified, then by this mixture twin-screw extrusion, granulation, then carries out drying, spinning.Publication number is the preparation method that the Chinese patent of CN101792938A discloses a kind of polyformaldehyde fibre, it adopts the polyformaldehyde spinning of melt index lower (MFR=1.8g/10min), poor for overcoming the too low fluidity of molten of melt index, be unfavorable for the winding of as-spun fibre, and adopt the method for multistage slow cooling, multistage stretching, with obtain uniformity better, Gao Mo, high-strength, stable performance fiber.Publication number is the melt-spinning technology that the Chinese patent of CN102011201A discloses a kind of polyformaldehyde fibre, it is by the method process as-spun fibre of slow cooling-quenching, crystallization control, preparation high strength polyformaldehyde fibre, the method selects the polyformaldehyde of different viscosities, hot solution water-bath pressurization is adopted to stretch, to obtain the polyformaldehyde fibre of high fracture strength.
Said method be all for current material propose improvement or improve existing technique, to make existing process matching in corresponding material, it all has some limitations, the matching of the relative different material of the technology provided is poor, and complex process, production efficiency is low, and cost is higher, and marketing and the application of its product are greatly limited.
Summary of the invention
The technical problem that the present invention solves is the preparation method providing a kind of polyformaldehyde fibre, and preparation method's applicability that the application provides is wide, can improve the mobility of polyformaldehyde matrix, and improves polyformaldehyde fibre mechanical property.
In view of this, this application provides a kind of preparation method of polyformaldehyde fibre, comprising:
Mixed with in-lubricant by acetal resin, extrude rear pelletizing, then carry out drying, then spinning, obtains polyformaldehyde fibre;
Described in-lubricant be selected from fatty acid ester in-lubricant, aliphatic alcohols in-lubricant, fatty acyl amide in-lubricant and low molecular weight hydrocarbons in-lubricant one or more.
Preferably, the melt index of described acetal resin is 0.5 ~ 15g/10min, and weight average molecular weight is 12 ~ 800,000.
Preferably, the melt index of described acetal resin is 1.0 ~ 9.0g/10min, and weight average molecular weight is 25 ~ 500,000.
Preferably, the weight average molecular weight of described in-lubricant is 1000 ~ 50000.
Preferably, the weight average molecular weight of described in-lubricant is 2000 ~ 10000.
Preferably, the mass ratio of described in-lubricant and acetal resin is (0.01 ~ 4.0): 100.
Preferably, the mass ratio of described in-lubricant and acetal resin is (0.5 ~ 2.0): 100.
Preferably, the temperature of described drying is 100 ~ 110 DEG C, and the time is 2 ~ 4h.
This application provides a kind of preparation method of polyformaldehyde fibre, acetal resin mixes with in-lubricant by it, extrudes rear pelletizing, then carries out drying, and then melt spinning, obtains polyformaldehyde fibre; Described in-lubricant be selected from fatty acid ester in-lubricant, aliphatic alcohols in-lubricant, fatty acyl amide in-lubricant and low molecular weight hydrocarbons in-lubricant one or more.This application provides a kind of preparation method of polyformaldehyde fibre, it by adding interior lubricating grease auxiliary agent in acetal resin, make it can not only improve the mobility of acetal resin matrix, and delay or suppress the crystallization of acetal resin, improve its crystal property, to reach the object of preparation spinnability excellence, high strength polyformaldehyde fibre; Preparation method of the present invention does not impact original polyformaldehyde production line and products thereof simultaneously, to instrument and supplies without particular/special requirement, has universality.
Detailed description of the invention
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of preparation method of polyformaldehyde fibre, comprising:
Mixed with in-lubricant by acetal resin, extrude rear pelletizing, then carry out drying, then spinning, obtains polyformaldehyde fibre;
Described in-lubricant be selected from fatty acid ester in-lubricant, aliphatic alcohols in-lubricant, fatty acyl amide in-lubricant and low molecular weight hydrocarbons in-lubricant one or more.
The application is in the process preparing polyformaldehyde fibre, by adding in-lubricant auxiliary agent in acetal resin, can improve the mobility of resin matrix, and reduce crystallization temperature, delay crystallization time, result shows that it is excellent to preparation spinnability, high strength polyformaldehyde fibre successful.
In the process preparing polyformaldehyde fibre, acetal resin directly mixes with in-lubricant by the application.For acetal resin, general melt index is larger, and molecular weight is lower, and melt index is less, and molecular weight is higher; Described in the application, the melt index of acetal resin is preferably 0.5 ~ 15g/10min, in certain embodiments, the melt index of described acetal resin is more preferably 1.0 ~ 9.0g/10min, and in certain embodiments, the melt index of described acetal resin is more preferably 2.0 ~ 5.0g/10min.Described in the application, the melt index of acetal resin is excessive, on then producing, the requirement of raw material, technique and device is increased, finally make cost increase, the requirement of production to raw material and technique of high molecular weight polyoxymethylene resin is more strict, and conversion ratio and product quality also can be subject to certain impact; Melt index is too small, then the intensity of the polyformaldehyde fibre prepared reduces.Described in the application, the weight average molecular weight of acetal resin is preferably 120,000 ~ 800,000, and in an embodiment, the weight average molecular weight of described acetal resin is more preferably 250,000 ~ 500,000.Described acetal resin can be the section of acetal resin, and also can be the powder of the acetal resin after polymerization, the state of the application to acetal resin limit especially.
In-lubricant described in the application be selected from fatty acid ester in-lubricant, aliphatic alcohols in-lubricant, fatty acyl amide in-lubricant and low molecular weight hydrocarbons in-lubricant one or more.In an embodiment, described in-lubricant is more preferably fatty acyl amide in-lubricant and low molecular weight hydrocarbons in-lubricant.Described in the application, the weight average molecular weight of in-lubricant is preferably 1000 ~ 50000, and in an embodiment, the weight average molecular weight of described in-lubricant is more preferably 2000 ~ 10000.Described in the application, the weight average molecular weight of in-lubricant decides the height of lubricant effect, molecular weight is too low, because of himself physicochemical property, as the impact of the factor such as boiling point, fusing point, in process, (melt extrude granulation, melt spinning) separate out, and lose its function; The compatibility of molecular weight too high then itself and acetal resin molecule is not good enough, in it lubricity be mainly reflected in be embedded in high molecular weight polyoxymethylene strand between play certain lubricant effect, make mutually slide between polyformaldehyde strand.The addition of in-lubricant described in the application is the 0.01wt% ~ 0.4wt% of described acetal resin, in an embodiment, is more preferably 0.5wt% ~ 2.0wt%.The addition of described in-lubricant determines the mobility preparing polyformaldehyde fibre, and addition is too small, then Resin Flow is low, and in preparation process, spinnability reduces, and cannot stretch under the low or equal conditions of after-drawing fibre strength; The addition of described in-lubricant is excessive, then the mobility of resin is too high, and drawing-off cannot be carried out.In-lubricant described in the application is well known to those skilled in the art, does not limit especially herein.
According to the present invention, after described acetal resin mixes with described in-lubricant, then the mixture obtained is extruded rear pelletizing, spinning after dry, obtains polyformaldehyde fibre.In above process, extrude with the process of described spinning described in be all modes well known to those skilled in the art, no longer to repeat herein.Described dry that temperature is preferably 100 ~ 110 DEG C, the time is preferably 2 ~ 4h.
Acetal resin mixes with outer interpolation in-lubricant by the preparation method of the application's polyformaldehyde fibre, through melt extruding after mixing, dry after pelletizing, and spinning.Preparation method of the present invention does not impact original polyformaldehyde production line and products thereof, to instrument and supplies without particular/special requirement, especially the polymerization process in polyformaldehyde production, namely under same raw material and technique, by mobility and the crystalline improvement of granulation process resin matrix, existing product and special polyformaldehyde spinning just can be obtained; Simultaneously, be different from fiber processing procedure and existingly compared with the technique being suitable for different viscosities resin by after-drawing process adjustments, the flexibility of the method is higher, it only needs the adjustment by in-lubricant, the mobility of different viscosities resin can be changed, reach and be applicable to existing or fixing fiber process apparatus and technique.Thus, the method is easy and simple to handle, cost is low, and its industrial utility value is high, applied widely, and limitation is little.
The application's in-lubricant and polyformaldehyde compatibility good, can to improve liquidity and crystalline in-lubricant can be low-molecular-weight hydro carbons, also can be other auxiliary agent of effects equivalent, as one or both and above composition of fatty acid ester, aliphatic alcohols, fatty acid amide, fat soap, this invention aims to provide a kind of method, is namely different from the structural adjustment of resin raw material and the rear making technology of different viscosities polyformaldehyde fibre; Moreover addition manner and the operation of in-lubricant are unrestricted, it can be the section of acetal resin, also can be the powder of the acetal resin after polymerization.
In order to understand the present invention further, below in conjunction with embodiment, the preparation method to polyformaldehyde fibre provided by the invention is described in detail, and protection scope of the present invention is not limited by the following examples.
Raw material in following examples is commercially available prod.
Following embodiment and comparative example adopt following methods to carry out comparative evaluation:
(1) melt index, Thermo company MT melting means instrument
Dried polyoxymethylene granulate or the powder preheating 5min at 190 DEG C processed, test by ISO1133 standard under load 2160g condition;
(2) crystal property test, U.S. TA company Q200 differential scanning calorimeter
Test condition: constant temperature 5min after nitrogen atmosphere lower 20 DEG C/min heating rate is warming up to 200 DEG C; Constant temperature 5min after being cooled to 90 DEG C with the speed of 10 DEG C/min; Again with the ramp to 200 DEG C of 10 DEG C/min, indicate crystallization half-peak breadth and crystallization initiation temperature by fusion-crystallization curve;
(3) molecular weight and distribution tests thereof, Japanese eastern Cao's science and technology HLC-8320GPC coagulant liquid chromatography
At 40 DEG C, the flow velocity of sample flow path is 0.5ml/min, and reference stream is set as 1/2 of sample flow rate, the weight average/number-average molecular weight of test polymer and distribution thereof, and Mw refers to mean molecule quantity;
(4) spinning equipment and technique
Singe screw melt spinning testing machine, screw diameter 20mm, draw ratio is 25:1, and compression ratio is 3:1, and spinnerets specification: 18 × 0.4mm, spinning technique refers to table 2.
Embodiment 1
Copolymerized methanal resin slicer A to be cut into slices 100 weight portions, add in-lubricant 0.5 weight portion again, in high-speed mixer and mixing 1min, extrude (expressing technique is as shown in table 1) through double screw extruder, through removing moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Spinning (spinning technique is as shown in table 2) is carried out in dried section on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C; In the present embodiment, the melt index of copolymerized methanal resin is 27.5g/10min, Mw is 136589, in-lubricant fatty acyl amide and the low molecular weight hydrocarbons in-lubricant of in-lubricant to be mass ratio be 1:1.
Embodiment 2
Copolymerized methanal resin slicer B to be cut into slices 100 weight portions, add in-lubricant 0.5 weight portion again, in high-speed mixer and mixing 1min, extrude (expressing technique is as shown in table 1) through double screw extruder, remove moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Spinning (spinning technique is as shown in table 2) is carried out in dried section on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C; In the present embodiment, the melt index of copolymerized methanal is 9.0g/10min, Mw is 203482, in-lubricant fatty acyl amide and the low molecular weight hydrocarbons in-lubricant of in-lubricant to be mass ratio be 1:1.
Embodiment 3
Copolymerized methanal resin slicer C to be cut into slices 100 weight portions, add in-lubricant 0.5 weight portion again, in high-speed mixer and mixing 1min, extrude (expressing technique is as shown in table 1) through double screw extruder, remove moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Spinning (spinning technique is as shown in table 2) is carried out in dried section on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C; The melt index of the present embodiment copolymerized methanal is 2.5g/10min, Mw is 286543, in-lubricant fatty acyl amide and the low molecular weight hydrocarbons in-lubricant of in-lubricant to be mass ratio be 1:1.
Embodiment 4
Copolymerized methanal resin slicer C to be cut into slices 100 weight portions, add in-lubricant 1.0 weight portion again, in high-speed mixer and mixing 1min, extrude (expressing technique is as shown in table 1) through double screw extruder, remove moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Spinning (spinning technique is as shown in table 2) is carried out in dried section on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C; The melt index 2.5g/10min of the present embodiment copolymerized methanal, Mw are 286543, in-lubricant fatty acyl amide and the low molecular weight hydrocarbons in-lubricant of in-lubricant to be mass ratio be 1:1.
Embodiment 5
Copolymerized methanal resin slicer C to be cut into slices 100 weight portions, add in-lubricant 2.0 weight portion again, in high-speed mixer and mixing 1min, extrude (expressing technique is as shown in table 1) through double screw extruder, remove moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Spinning (spinning technique is as shown in table 2) is carried out in dried section on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C; The melt index of the present embodiment copolymerized methanal is 2.5g/10min, Mw is 286543, in-lubricant fatty acyl amide and the low molecular weight hydrocarbons in-lubricant of in-lubricant to be mass ratio be 1:1.
Comparative example 1
By copolymerized methanal resin slicer A, extrude (expressing technique is as shown in table 1) through double screw extruder, remove moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Dried section carries out spinning (spinning technique is as shown in table 2) on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C.
Comparative example 2
By copolymerized methanal resin slicer B, extrude (expressing technique is as shown in table 1) through double screw extruder, remove moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Dried section carries out spinning (spinning technique is as shown in table 2) on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C.
Comparative example 3
Copolymerized methanal resin slicer C is extruded (expressing technique is as shown in table 1) through double screw extruder, removes moisture at 105 DEG C of dry 3h after pelletizing, carry out the test of melt index and crystal property; Dried section carries out spinning (spinning technique is as shown in table 2) on singe screw melt spinning machine, and spinning screw temperature, assembly and pipe temperature are 200 DEG C, after-drawing heat roller temperature 120 DEG C.
Table 1 embodiment and comparative example procession parameters table
Table 2 embodiment and comparative example spinning technology parameter table
The tables of data of polyformaldehyde fibre prepared by table 3 embodiment and comparative example
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (8)

1. a preparation method for polyformaldehyde fibre, comprising:
Mixed with in-lubricant by acetal resin, extrude rear pelletizing, then carry out drying, then spinning, obtains polyformaldehyde fibre;
Described in-lubricant be selected from fatty acid ester in-lubricant, aliphatic alcohols in-lubricant, fatty acyl amide in-lubricant and low molecular weight hydrocarbons in-lubricant one or more.
2. preparation method according to claim 1, is characterized in that, the melt index of described acetal resin is 0.5 ~ 15g/10min, and weight average molecular weight is 12 ~ 800,000.
3. preparation method according to claim 2, is characterized in that, the melt index of described acetal resin is 1.0 ~ 9.0g/10min, and weight average molecular weight is 25 ~ 500,000.
4. preparation method according to claim 1, is characterized in that, the weight average molecular weight of described in-lubricant is 1000 ~ 50000.
5. preparation method according to claim 1, is characterized in that, the weight average molecular weight of described in-lubricant is 2000 ~ 10000.
6. preparation method according to claim 1, is characterized in that, the mass ratio of described in-lubricant and acetal resin is (0.01 ~ 4.0): 100.
7. preparation method according to claim 1, is characterized in that, the mass ratio of described in-lubricant and acetal resin is (0.5 ~ 2.0): 100.
8. preparation method according to claim 1, is characterized in that, the temperature of described drying is 100 ~ 110 DEG C, and the time is 2 ~ 4h.
CN201510955587.6A 2015-12-17 2015-12-17 Polyformaldehyde fiber preparation method Pending CN105386151A (en)

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CN106480535A (en) * 2016-10-31 2017-03-08 江苏苏博特新材料股份有限公司 A kind of method that polyformaldehyde fibre prepared by melt spinning
CN113201220A (en) * 2021-05-08 2021-08-03 广州搜料信息技术有限公司 PPS polyphenylene sulfide modified polymer modified by short fibers and preparation process thereof
CN115679686A (en) * 2022-10-21 2023-02-03 山东鲁化森萱新材料有限公司 High-performance polyformaldehyde fiber for concrete and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106480535A (en) * 2016-10-31 2017-03-08 江苏苏博特新材料股份有限公司 A kind of method that polyformaldehyde fibre prepared by melt spinning
CN113201220A (en) * 2021-05-08 2021-08-03 广州搜料信息技术有限公司 PPS polyphenylene sulfide modified polymer modified by short fibers and preparation process thereof
CN115679686A (en) * 2022-10-21 2023-02-03 山东鲁化森萱新材料有限公司 High-performance polyformaldehyde fiber for concrete and preparation method thereof

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