CN102093694A - Polyacrylonitrile pulp master batch - Google Patents
Polyacrylonitrile pulp master batch Download PDFInfo
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- CN102093694A CN102093694A CN2009102019266A CN200910201926A CN102093694A CN 102093694 A CN102093694 A CN 102093694A CN 2009102019266 A CN2009102019266 A CN 2009102019266A CN 200910201926 A CN200910201926 A CN 200910201926A CN 102093694 A CN102093694 A CN 102093694A
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Abstract
The invention relates a method for preparing a polyacrylonitrile pulp master batch, and belongs to the technical field of functional high polymer materials. The method comprises the following steps of: adsorbing functional inorganic powder which is pretreated by a high-efficiency coupling agent uniformly by utilizing the high-capturing performance of high fibrillating polyacrylonitrile pulp under the action of high shear, so that microfibers of the polyacrylonitrile pulp are isolated effectively and have high compatibility with a matrix; and mixing matrix thermoplastic elastomer particles or powder and an isolated pulp complex fully, and forming a composite master batch containing 25 to 40 percent of polyacrylonitrile pulp under the appropriate processing condition. In the method, an organic solvent which is adverse to the environment is not used, the polyacrylonitrile pulp in the prepared master batch is uniformly distributed and can be applied to reinforcing systems of different high polymer matrixes directly; and a process is simple and flexible and is low in cost.
Description
Technical field
The invention belongs to functional high molecule material manufacturing technology field.The manufacture method that relates to a kind of polyacrylonitrile master batch specifically relates to a kind of high acquisition performance that utilizes height primary fibrosis polypropylene nitrile pulp, makes the method for high-content polyacryl-nitrile dissolving pulp master batch.
Technical background
As everyone knows, fibrous magnesium silicate is a kind of inorganic fibers that has fire-retardant, enhancing, thixotroping concurrently, helps excellent over-all propertieies such as processing, often be widely used in multiple fields such as friction materials, sealing material, material of construction, but no matter the fibrous magnesium silicate goods all can cause serious harm to HUMAN HEALTH in producing or using, thereby the countries in the world scientific research personnel is being devoted to seek a kind of novel non-asbestos fiber to substitute existing fibrous magnesium silicate.
" golden spider " card series p-aramid fiber pulp and " beautiful spider " card series polyacryl-nitrile dissolving pulp of the exploitation of the blue nation in Kevlar Pulp, Twaron Pulp that Dupont, Japanese Supreme Being people company take the lead in developing and Shanghai are the ideal products that replaces fibrous magnesium silicate.And the dissolving pulp-like fibre similar is promptly adhered to many fentos on every branch bar in dendroid, and surface hairiness is very abundant, and therefore, specific surface area is huge, and (specific surface area of general chopped strand has only 0.1～1m
2/ g, the pulp specific surface area reaches 10～25m
2/ g), be used for matrix material, have the very strong ability of catching fine particle, constituents for suppressing loss.And the fibrous texture of this uniqueness, be that the trunk fiber surface is the lint shape, axially the tail end fibril changes into tip-like, make and take place easily between the fiber to tangle and difficult being distributed to equably in the matrix of matrix material, making the fiber with this excellent structural performance can not give full play to it should have effect, and restricts its Application Areas greatly.
For this reason, du pont company (USP 4514541) has proposed to utilize the prescription and the preparation technology of elastomer solution and p-aramid fiber pulp and reinforcement elastomerics mixed together uniform preparation aramid pulp granular elastomer rubber master batch, the rubber master batch that contains 20% aramid pulp of preparation has good dispersiveness in elastomer matrix, the normal temperature of its enhanced elastic composite and drawing by high temperature mechanical performance index improve a lot, this process using need adopt a large amount of contaminative organic solvent toluene, thereby brings disadvantageous effect for security and the environment produced.As replenishing and development of above-mentioned technology, E.I.Du Pont Company (EP 0272459) discloses prescription and the preparation technology who utilizes liquid elastomer and aramid pulp and reinforced filling to prepare aramid pulp granular elastomer rubber master batch again, the rubber master batch that contains 10% aramid pulp of preparation has good dispersiveness in elastomer matrix, the stress ratio under its enhanced elastic composite small deformation directly uses aramid pulp enhanced elastic composite to exceed 50-200%.
As can be seen, the above-mentioned technology of E.I.Du Pont Company is subjected to the restriction of solvent contamination and liquid elastomer kind, can't be applicable to the matrices of composite material of many kinds, and cost is very high, can not give full play to the enhancing potentiality of p-aramid fiber pulp.
For this reason, China Beijing University of Chemical Technology (CN 200510083844.8) has proposed a kind of pretreatment process of p-aramid fiber pulp, utilize hollow glass micropearl as inorganic isolation powder with mix the mixture that forms the p-aramid fiber pulp with phthalate compound again after loose p-aramid fiber pulp mixes as lubricant, can make p-aramid fiber pulp dispersing property excellence in elastomerics, help improving the performance of its enhanced elastic composite, particularly this method has avoided making the organic solvent of land used environmental pollution.But this method is used a large amount of phthalate lubricants, and final residue will influence the performance of goods in compound system, and this treatment process does not still break through the p-aramid fiber pulp only in the application in rubber elastomer field simultaneously.
The blue CN 200910057137.X of nation in Shanghai has proposed not use any to the disadvantageous organic solvent of environment, the p-aramid fiber pulp is evenly distributed in the compound parent that makes, can directly apply to the enhancing system of different matrix, comprise multiple fields such as engineering plastics and engineering rubber, technology is simple, flexible and cost is lower.
And arrive at present, there are light bubble, metering difficulty and are difficult for finely dispersed problem though polyacryl-nitrile dissolving pulp is same, relevant application technical research does not see that as yet report is arranged.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method of making the polyacryl-nitrile dissolving pulp master batch, pulp is uniformly dispersed in different application matrixes, effectively improve the enhancing potentiality of polyacryl-nitrile dissolving pulp in matrix material, and technology is simple, flexible and pollution-free.
Technical scheme of the present invention is: the high acquisition performance that utilizes height primary fibrosis polypropylene nitrile pulp, under high shear forces, evenly absorption is through the efficient pretreated function inorganic powder of coupling agent, make form between the fento of polyacryl-nitrile dissolving pulp effectively isolate and with strengthen matrix good consistency arranged, again with thermoplastic elastic particle or powder and after the pulp mixture of isolation processing carries out thorough mixing, select suitable processing conditions for use according to the characteristic of different matrix, form the master batch that contains p-aramid fiber pulp 25～40%.
The present invention has the following advantages:
1. make full use of the high acquisition performance of height primary fibrosis polypropylene nitrile pulp, make the polyacryl-nitrile dissolving pulp master batch, do not use the organic solvent of any environmental pollution or contain the component that lowers enhancing system performance impact;
Pre-treatment, polyacryl-nitrile dissolving pulp with the efficient coupling agent of inorganic powder disperse with the high-speed mixing of inorganic powder, thermoplastic elastic particle or powder with can in same equipment, finish through mixing of isolation processing polyacryl-nitrile dissolving pulp, simplified the manufacturing process treatment scheme greatly;
3. the polyacryl-nitrile dissolving pulp master batch of making can equally with common macromolecule raw material directly apply to the enhancing system, and application requiring lowers significantly;
Description of drawings
Fig. 1 is polyacryl-nitrile dissolving pulp photo figure in kind.
Fig. 2 is polyacryl-nitrile dissolving pulp master batch of the present invention photo in kind.
Embodiment
The technical characterictic of polyacryl-nitrile dissolving pulp master batch manufacture method of the present invention is: height primary fibrosis polypropylene nitrile pulp evenly adsorbs through the pretreated function inorganic powder of efficient coupling agent, make form between the fento of polyacryl-nitrile dissolving pulp effectively isolate and with strengthen matrix good consistency arranged, again with thermoplastic elastic particle or powder and after the pulp mixture of isolation processing carries out thorough mixing, select suitable processing conditions for use according to the characteristic of different matrix, form the master batch that contains polyacryl-nitrile dissolving pulp 25～40%.
Function inorganic powder of the present invention can be wherein one or more such as inorganic non-metallic mineral powder such as lime carbonate, barium sulfate, talcum powder, wollastonite, glass microballon;
Efficient coupling agent of the present invention can be silicane, titanate ester or aluminium esters of gallic acid coupling agent, preferably requires to select for use metatitanic acid acids coupling agent according to system;
Coupling agent of the present invention can adopt direct premixed method to inorganic functional powder pre-treating method, but better method is in high-efficiency mixing device, inorganic powder is in high-speed stirring, and the vaporific coupling agent that sprays into makes a small amount of coupling agent can be coated on the surface of inorganic powder equably;
Polyacryl-nitrile dissolving pulp of the present invention carries out the high-shear dispersing and mixing with the inorganic functional powder that is evenly cladded by efficient coupling agent in high-efficiency mixing device, form effective isolation system of polyacryl-nitrile dissolving pulp;
Thermoplastic elastic particle of the present invention or powder can be matrixes such as TPE, TPO, EVM, EVA, TPU, POE;
The enforcement of high efficient mixed process of the present invention can be finished in same high shear mixing equipment, inside comprises the orthogonal double-deck whipping appts of two covers, lower floor is high rotating speed sheet structure, dissolving pulp-like fibre is fully stretched under high shear forces, and powder can evenly be adsorbed, and low speed oar formula structure is adopted on the upper strata, make centrifugal upwards and the material on the limit in equipment, stir to the center downwards, with form thorough mixing, equally distributed stable complex is;
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.
The polyacryl-nitrile dissolving pulp that adopts is " beautiful spider " JLP-502 type that Shanghai Lanbang Industry Fibre Co., Ltd. produces among the embodiment, and its technical indicator is: length distribution 1.8 ± 0.4mm; Specific surface area is 12.9m
2/ g, its photo in kind as shown in Figure 1.
High shear mixing equipment is self design, cover and have the liquid spray feeding device, inside comprises the orthogonal double-deck whipping appts of two covers, lower floor is high rotating speed sheet structure, dissolving pulp-like fibre is fully stretched under high shear forces, and powder can evenly be adsorbed, and low speed oar formula structure is adopted on the upper strata, make centrifugal upwards and the material on the limit in equipment, stir to the center downwards.
Example 1
In high shear mixing equipment, add 1000 order fine active light calcium carbonate 1500g, spraying adds monoalkoxy type titanate coupling agent 15g in high-speed stirring, make it be coated on the outside of lime carbonate equably, add polyacryl-nitrile dissolving pulp 1500g then, high-speed stirring starts low speed simultaneously and stirs again, after thorough mixing is even, add polyolefin elastomer particle POE1285g, continuation high-speed stirring, low speed stir, and form the even compound system that contains polyacryl-nitrile dissolving pulp.After the discharging, adopt the forced feed device, through direct twin screw extruder granulating system, forming with POE is the master batch that matrix contains polyacryl-nitrile dissolving pulp 35%.
Example 2
In high shear mixing equipment, add 1000 order fine active light calcium carbonate 1500g, spraying adds monoalkoxy type titanate coupling agent 15g in high-speed stirring, make it be coated on the outside of lime carbonate equably, add polyacryl-nitrile dissolving pulp 1500g then, high-speed stirring starts low speed simultaneously and stirs again, after thorough mixing is even, add vinyl-acetic ester rubber particles EVM750g, continuation high-speed stirring, low speed stir, and form to contain the compound system of polyacryl-nitrile dissolving pulp.After the discharging, adopt the forced feed device, through direct twin screw extruder granulating system, forming with EVM is that matrix contains polyacryl-nitrile dissolving pulp 40% master batch.
Example 3
In high shear mixing equipment, add 1000 order fine active light calcium carbonate 1500g, spraying adds monoalkoxy type titanate coupling agent 15g in high-speed stirring, make it be coated on the outside of lime carbonate equably, add polyacryl-nitrile dissolving pulp 1500g then, high-speed stirring starts low speed simultaneously and stirs again, after thorough mixing is even, add polyurethane termoplastic elastomer 750g, continuation high-speed stirring, low speed stir, and form to contain the compound system of p-aramid fiber.After the discharging, adopt the forced feed device, through direct twin screw extruder granulating system, forming with TPU is the master batch that matrix contains polyacryl-nitrile dissolving pulp 40%.
Claims (9)
1. the manufacture method of a polyacryl-nitrile dissolving pulp master batch.It is characterized in that: height primary fibrosis polypropylene nitrile pulp evenly adsorbs through the pretreated function inorganic powder of efficient coupling agent, make to form between the fento of pulp and effectively isolate and good consistency is arranged with matrix, again with matrix thermoplastic elastomer particle or powder and after the pulp mixture of isolation processing carries out thorough mixing, select suitable processing conditions for use, form the composite master batch that contains polyacryl-nitrile dissolving pulp 25～40%.
2. method according to claim 1 is characterized in that: described function inorganic powder can be wherein one or more such as inorganic non-metallic mineral powder such as lime carbonate, barium sulfate, talcum powder, wollastonite, glass microballon.
3. method according to claim 1 is characterized in that: described efficient coupling agent can be silicane, titanate ester or aluminium esters of gallic acid coupling agent, preferably requires to select for use metatitanic acid acids coupling agent according to system.
4. method according to claim 1, it is characterized in that: described coupling agent can adopt direct premixed method to inorganic functional powder pre-treating method, but better method is in high-efficiency mixing device, inorganic powder is in high-speed stirring, the vaporific coupling agent that sprays into makes a small amount of coupling agent can be coated on the surface of inorganic powder equably.
5. according to claim 1 and 4 described methods, it is characterized in that: described polyacryl-nitrile dissolving pulp carries out the high-shear dispersing and mixing with the inorganic functional powder that is evenly cladded by efficient coupling agent in high-efficiency mixing device, form effective isolation system of polyacryl-nitrile dissolving pulp.
6. method according to claim 1 is characterized in that: described thermoplastic elastomer particle or powder can be matrixes such as TPE, TPO, EVM, TPU, EVA, POE;
7. method according to claim 1 is characterized in that: described thermoplastic elastic particle or powder and polyacryl-nitrile dissolving pulp are isolated system and are carried out abundant dispersing and mixing, form stabilized complex.
8. according to claim 1,4,5 and 7 described methods, it is characterized in that: the enforcement of described high efficient mixed process can be finished in same high shear mixing equipment, inside comprises the orthogonal double-deck whipping appts of two covers, lower floor is high rotating speed sheet structure, dissolving pulp-like fibre is fully stretched under high shear forces, and powder can evenly be adsorbed, and low speed oar formula structure is adopted on the upper strata, make centrifugal upwards and the material on the limit in equipment, stir to the center downwards, with form thorough mixing, equally distributed stable complex is;
9. according to claim 1 and 7 described methods, it is characterized in that: described mixture is selected suitable processing conditions for use according to the characteristic of different matrix, utilize the forced feed device,, form the master batch that contains polyacryl-nitrile dissolving pulp 25～40% through the twin screw extruder granulating system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102019266A CN102093694A (en) | 2009-12-14 | 2009-12-14 | Polyacrylonitrile pulp master batch |
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|---|---|---|---|
| CN2009102019266A CN102093694A (en) | 2009-12-14 | 2009-12-14 | Polyacrylonitrile pulp master batch |
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| CN102093694A true CN102093694A (en) | 2011-06-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110528272A (en) * | 2019-09-16 | 2019-12-03 | 武汉纺织大学 | A kind of polyimide fiber fibrillation treatment method |
-
2009
- 2009-12-14 CN CN2009102019266A patent/CN102093694A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110528272A (en) * | 2019-09-16 | 2019-12-03 | 武汉纺织大学 | A kind of polyimide fiber fibrillation treatment method |
| CN110528272B (en) * | 2019-09-16 | 2021-09-17 | 武汉纺织大学 | Polyimide fiber fibrillation treatment method |
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Addressee: You Xiulan Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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Addressee: Shanghai Lanbang Industrial Fiber Co Ltd You Xiulan Document name: Notification of before Expiration of Request of Examination as to Substance |
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Addressee: Shanghai Lanbang Industry Fibre Co., Ltd. Document name: Notification that Application Deemed to be Withdrawn |
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Application publication date: 20110615 |