CN103538348B - A kind of manufacture method of flame retardant rubber - Google Patents
A kind of manufacture method of flame retardant rubber Download PDFInfo
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- CN103538348B CN103538348B CN201310431011.0A CN201310431011A CN103538348B CN 103538348 B CN103538348 B CN 103538348B CN 201310431011 A CN201310431011 A CN 201310431011A CN 103538348 B CN103538348 B CN 103538348B
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Abstract
The invention discloses a kind of manufacture method of flame retardant rubber, relate to rubber and manufacture field, by plasticating, mixing, shaping, process, gluing, glue connects and dries the preparation that seven steps complete flame retardant rubber, in the flame retardant rubber of this preparation, first plasticate, improve the plasticity of rubber, in step below, rubber can mix well with other materials, with the addition of acetonitrile rubber, add ductility, in forming step, in vacuum environment, cool drying 24h under 25 DEG C of conditions, vacuum condition can slough the bubble in mixed glue, Slow cooling under normal temperature, colloid is not easily made to occur crackle when drying, make its more consolidation, the effectiveness that the employing of polyurethane film mainly take into account neoprene is better, but mid portion more easily consumes than two end portions, increase two panels polyurethane film and extend flame retardant rubber service life.
Description
Technical field
The present invention relates to rubber and manufacture field, particularly relate to a kind of manufacture method of flame retardant rubber.
Background technology
Rubber (Rubber): the strong flexible polymer material with reversible deformation.At room temperature high resilience, can produce comparatively large deformation under very little External Force Acting, resilient after removing external force.Rubber belongs to complete amorphous polymer, and its glass transition temperature (Tg) is low, molecular weight is often very large, and be greater than hundreds of thousands, neoprene take chlorobutadiene as primary raw material, by homopolymerization or other monomer copolymerization on a small quantity.As tensile strength is high, heat-resisting, fast light, ageing-resistant performance is excellent, oil resistance is all better than natural rubber, butadiene-styrene rubber, butadiene rubber.Have stronger flame resistance and excellent fire retardance, its chemical stability is higher, and resistance to water is good.The shortcoming of neoprene is electrical insulation capability, and cold tolerance is poor, and rubber is unstable when storing, and when being used for manufacturing the flame retardant rubber for centrifugal pump or diaphragm pump in thin pulp transport, service life is low, and ductility is bad, and the present invention changes these shortcomings.
Summary of the invention
For overcoming the deficiency in prior art, the object of the invention is to provide a kind of manufacture method thickening durable flame retardant rubber.
For realizing object of the present invention, technical scheme of the present invention is as follows:
A manufacture method for flame retardant rubber, its processing step is as follows:
(1) plasticate: get neoprene fecula 80g, acrylonitrile-butadiene rubber fecula 20g plasticates;
(2) mixing: in the fourth rubber fecula of plasticating and acrylonitrile-butadiene rubber fecula, to add carbon black 30g, short fiber 10g, stearic acid 1g, nano flame retardant compound 10-15g; It is 8MPa that antiager 1.5g and altax 43.5 ~ 4.5g carries out mixing condition in mixing roll, 150 ~ 190 DEG C, 20min; The preparation method of described nano flame retardant complexing agent is:
A silicone hydroxyl apatite, red phosphorus, concave convex rod, hydrotalcite, imvite, titanium dioxide, calcite, kaolin mix according to the mass fraction proportioning of 25-35:15-20:10-15:10-15:8-10:8-10:7-8:5-7 by (), join in the mixed solution of 200 parts of methyl-sulfoxides (DMSO) and 50 parts of methyl alcohol, stir 60 hours in 65 DEG C, filter, and wash the excessive methyl-sulfoxide (DMSO) of 3 removings with the hot ethanol of 60 DEG C of temperature, put into vacuum drying chamber, 60 DEG C of temperature dryings 24 hours, grinding is sieved, and obtains a modified flame-retardant compound;
(b), by the mixing of 1 part of modified flame-retardant compound, 10 parts of potassium acetates and 25 parts of distilled water, more than 10 hours are stirred in temperature 50 C, in temperature 30 DEG C, first disperse 2.5 hours under ultrasonic electric power 350W condition, and then disperse 3 hours under ultrasonic electric power 250W condition.To filter, and with distilling washing 3 times, 80 DEG C of vacuum drying 24 hours, grinding is sieved, and obtains twice-modified flame-retardant compounds;
(c), by above-mentioned 1 part of twice-modified flame-retardant compounds at 600W power ultrasonic dispersion 40min, be heated to 90 DEG C with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical agitator; Obtain nano flame retardant compound;
(3) shaping: mixing gained to be melted slurry and take advantage of heat to pour in mould, in vacuum environment, cool drying 24h under 25 DEG C of conditions, the flame retardant rubber of system;
(4) process: get two panels 0.1mm polyurethane film, use methyl alcohol, isopropyl alcohol and acetonitrile mixture ultrasonic degreasing 3 ~ 5min respectively, after clean by washed with de-ionized water, use acetone wiping, for subsequent use;
(5) gluing: temperature be 25 DEG C, relative air humidity is less than in the operating room of 70%, with gasoline by 0.1mm polyurethane film surface clean one time, first dip a small amount of isocyanate glue to wave at gasoline and smear one deck to time half-dried, carry out pregelatinated, then etc. gasoline all volatilize the uniform isocyanate glue of rear painting last layer;
(6) glue connects: the polyurethane film of gluing is affixed on flame retardant rubber two sides center position;
(7) dry: be placed in 40 DEG C of baking ovens and dry 10min.
The manufacture method of above-mentioned a kind of flame retardant rubber, wherein, in (3) step, in isopropyl alcohol and acetonitrile mixture, the volume ratio of isopropyl alcohol and acetonitrile is 1:1.
The manufacture method of above-mentioned a kind of flame retardant rubber, wherein, the 0.1mm polyurethane film in (4) step is the circular membrane of diameter 2cm.
The manufacture method of above-mentioned a kind of flame retardant rubber, wherein, in (5) step, the thickness of isocyanate glue is 0.08mm thickness.
Beneficial effect of the present invention: by plasticating, mixing, shaping, process, gluing, glue connects and dries the preparation that seven steps complete flame retardant rubber, in the flame retardant rubber of this preparation, first plasticate, improve the plasticity of rubber, in step below, rubber can mix well with other materials, with the addition of acetonitrile rubber, add ductility, in forming step, in vacuum environment, cool drying 24h under 25 DEG C of conditions, vacuum condition can slough the bubble in mixed glue, Slow cooling under normal temperature, colloid is not easily made to occur crackle when drying, make its more consolidation, the effectiveness that the employing of polyurethane film mainly take into account neoprene is better, but mid portion more easily consumes than two end portions, increase two panels polyurethane film and extend flame retardant rubber service life, the thickness of 0.01mm does not affect the use of flame retardant rubber yet, in gluing process, first dip a small amount of isocyanate glue to wave at gasoline and smear one deck to time half-dried, carry out pregelatinated, gasoline is waited all to volatilize the uniform isocyanate glue of rear painting last layer again, the viscosity of glue is played better, strengthen viscose glue ability.Fire retardant prepared by the present invention is not halogen-containing, organic matter, and asepsis environment-protecting, has a extensive future; The present invention carries out twice-modified, and such benefit is: increase reactivity point, improves modified effect; Can steam again except the moisture in system while modification, dry and modification is carried out simultaneously, improves operating efficiency; There is a large amount of physics and chemistry adsorbed water in self micropore such as nano silicone hydroxyapatite, concave convex rod, imvite, kaolin, at high temperature produce water vapour, block oxygen, absorb heat, reach multiple fire-retardant effect; Powerful absorption property effectively can improve the synergy of several fire retardant, stops and is raised by fire retardant matter temperature, improve flame retarding efficiency; The aboundresources such as silicone hydroxyl apatite, concave convex rod, imvite, kaolin, greatly reduces the industrial cost of fire retardant, also for the Application and Development of attapulgite provides a new way; The present invention adopt solwution method ultrasonic wave disperse and mechanical high-speed agitator stir, make fire retardant separately component reach nano-scale dispersion in the solution, effectively prevent the autoxidation to composite, thus make composite have better mechanical property.
Detailed description of the invention
The technological means realized for making the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with detailed description of the invention, setting forth the present invention further.
Embodiment 1:
A manufacture method for flame retardant rubber, its processing step is as follows:
(1) plasticate: get neoprene fecula 80g, acrylonitrile-butadiene rubber fecula 20g plasticates, improve its plasticity, the interpolation of acetonitrile rubber, adds ductility;
(2) mixing: in the fourth rubber fecula of plasticating and acrylonitrile-butadiene rubber fecula, to add carbon black 30g, short fiber 10g, stearic acid 1g, nano flame retardant compound 10-15g; It is 8MPa that antiager 1.5g and altax 43.5 ~ 4.5g carries out mixing condition in mixing roll, 150 ~ 190 DEG C, 20min; The preparation method of described nano flame retardant complexing agent is:
A silicone hydroxyl apatite, red phosphorus, concave convex rod, hydrotalcite, imvite, titanium dioxide, calcite, kaolin mix according to the mass fraction proportioning of 25-35:15-20:10-15:10-15:8-10:8-10:7-8:5-7 by (), join in the mixed solution of 200 parts of methyl-sulfoxides (DMSO) and 50 parts of methyl alcohol, stir 60 hours in 65 DEG C, filter, and wash the excessive methyl-sulfoxide (DMSO) of 3 removings with the hot ethanol of 60 DEG C of temperature, put into vacuum drying chamber, 60 DEG C of temperature dryings 24 hours, grinding is sieved, and obtains a modified flame-retardant compound;
(b), by the mixing of 1 part of modified flame-retardant compound, 10 parts of potassium acetates and 25 parts of distilled water, more than 10 hours are stirred in temperature 50 C, in temperature 30 DEG C, first disperse 2.5 hours under ultrasonic electric power 350W condition, and then disperse 3 hours under ultrasonic electric power 250W condition.To filter, and with distilling washing 3 times, 80 DEG C of vacuum drying 24 hours, grinding is sieved, and obtains twice-modified flame-retardant compounds;
(c), by above-mentioned 1 part of twice-modified flame-retardant compounds at 600W power ultrasonic dispersion 40min, be heated to 90 DEG C with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical agitator; Obtain nano flame retardant compound;
(3) shaping: mixing gained to be melted slurry and take advantage of heat to pour in mould, in vacuum environment, cool drying 24h under 25 DEG C of conditions, the flame retardant rubber of system, vacuum condition can slough the bubble in mixed glue, Slow cooling under normal temperature, not easily make colloid occur crackle when drying, make its more consolidation;
(4) process: get two panels 0.1mm polyurethane film, use methyl alcohol, isopropyl alcohol and acetonitrile mixture ultrasonic degreasing 5min respectively, after clean by washed with de-ionized water, use acetone wiping, for subsequent use, the employing of polyurethane film mainly take into account the effectiveness of neoprene better, but mid portion more easily consumes than two end portions, increase two panels polyurethane film and extend flame retardant rubber service life, the thickness of 0.01mm does not affect the use of flame retardant rubber yet;
(5) gluing: temperature be 25 DEG C, relative air humidity is less than in the operating room of 70%, with gasoline by 0.1mm polyurethane film surface clean one time, first dip a small amount of isocyanate glue to wave at gasoline and smear one deck to time half-dried, carry out pregelatinated, gasoline is waited all to volatilize the uniform isocyanate glue of rear painting last layer again, the viscosity of glue is played better, strengthen viscose glue ability;
(6) glue connects: the polyurethane film of gluing is affixed on flame retardant rubber two sides center position;
(7) dry: be placed in 40 DEG C of baking ovens and dry 10min.
The manufacture method of above-mentioned a kind of flame retardant rubber, wherein, in (3) step, in isopropyl alcohol and acetonitrile mixture, the volume ratio of isopropyl alcohol and acetonitrile is 1:1.
The manufacture method of above-mentioned a kind of flame retardant rubber, wherein, the 0.1mm polyurethane film in (4) step is the circular membrane of diameter 2cm.
The manufacture method of above-mentioned a kind of flame retardant rubber, wherein, in (5) step, the thickness of isocyanate glue is 0.08mm thickness.
In the manufacture method of this flame retardant rubber, by plasticating, mixing, shaping, process, gluing, glue connects and dries the preparation that seven steps complete flame retardant rubber, in the flame retardant rubber of this preparation, first plasticate, improve the plasticity of rubber, in step below, rubber can mix well with other materials, with the addition of acetonitrile rubber, add ductility, in forming step, in vacuum environment, cool drying 24h under 25 DEG C of conditions, vacuum condition can slough the bubble in mixed glue, Slow cooling under normal temperature, colloid is not easily made to occur crackle when drying, make its more consolidation, the effectiveness that the employing of polyurethane film mainly take into account neoprene is better, but mid portion more easily consumes than two end portions, increase two panels polyurethane film and extend flame retardant rubber service life, the thickness of 0.01mm does not affect the use of flame retardant rubber yet, in gluing process, first dip a small amount of isocyanate glue to wave at gasoline and smear one deck to time half-dried, carry out pregelatinated, gasoline is waited all to volatilize the uniform isocyanate glue of rear painting last layer again, the viscosity of glue is played better, strengthen viscose glue ability.Fire retardant prepared by the present invention is not halogen-containing, organic matter, and asepsis environment-protecting, has a extensive future; The present invention carries out twice-modified, and such benefit is: increase reactivity point, improves modified effect; Can steam again except the moisture in system while modification, dry and modification is carried out simultaneously, improves operating efficiency; There is a large amount of physics and chemistry adsorbed water in self micropore such as nano silicone hydroxyapatite, concave convex rod, imvite, kaolin, at high temperature produce water vapour, block oxygen, absorb heat, reach multiple fire-retardant effect; Powerful absorption property effectively can improve the synergy of several fire retardant, stops and is raised by fire retardant matter temperature, improve flame retarding efficiency; The aboundresources such as silicone hydroxyl apatite, concave convex rod, imvite, kaolin, greatly reduces the industrial cost of fire retardant, also for the Application and Development of attapulgite provides a new way; The present invention adopt solwution method ultrasonic wave disperse and mechanical high-speed agitator stir, make fire retardant separately component reach nano-scale dispersion in the solution, effectively prevent the autoxidation to composite, thus make composite have better mechanical property.
Embodiment 2: all the other are identical with described embodiment 1, and difference is, in (2) step, mixing condition is 8MPa, 100 DEG C, 1h, but at such temperature, time expand can not strengthen melting effect, and the mixed glue obtained is easy to crack.
Embodiment 3: all the other are identical with described embodiment 1, and difference is, in (5) step, the thickness of isocyanate glue is coated with thinner, and be of uniform thickness with pregelatinated, polyurethane film easily comes off.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize content of the present invention to do equivalent structure or the conversion of equivalent flow process, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. a manufacture method for flame retardant rubber, is characterized in that, its processing step is as follows:
Step one, to plasticate: get neoprene fecula 80g, acrylonitrile-butadiene rubber fecula 20g plasticates;
Step 2, mixing: in the fourth rubber fecula of plasticating and acrylonitrile-butadiene rubber fecula, to add carbon black 30g, short fiber 10g, stearic acid 1g, nano flame retardant compound 10-15g; Antiager 1.5g and 3.5 ~ 4.5g altax 4 carry out mixing in mixing roll, and mixing condition is 8MPa, 150 ~ 190 DEG C, 20min; The preparation method of described nano flame retardant compound is:
First: silicone hydroxyl apatite, red phosphorus, concave convex rod, hydrotalcite, imvite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15:10-15:8-10:8-10:7-8:5-7, join in the mixed solution of 200 parts of methyl-sulfoxide DMSO and 50 part methyl alcohol, stir 60 hours in 65 DEG C, filter, and wash the excessive methyl-sulfoxide DMSO of 3 removings with the hot ethanol of 60 DEG C of temperature, put into vacuum drying chamber, 60 DEG C of temperature dryings 24 hours, grinding is sieved, and obtains a modified flame-retardant compound;
Secondly: by 1 part of modified flame-retardant compound, 10 parts of potassium acetates and 25 parts of distilled water mixing, more than 10 hours are stirred in temperature 50 C, in temperature 30 DEG C, first disperse 2.5 hours under ultrasonic electric power 350W condition, and then disperse 3 hours under ultrasonic electric power 250W condition, filter, and with distilling washing 3 times, 80 DEG C of vacuum drying 24 hours, grinding is sieved, and obtains twice-modified flame-retardant compounds;
Last: by above-mentioned 1 part of twice-modified flame-retardant compounds at 600W power ultrasonic dispersion 40min, to be heated to 90 DEG C with constant temperature heating device, and to stir 60 minutes with mechanical agitator with the rotating speed of 1200r/min; Obtain nano flame retardant compound;
Step 3, shaping: mixing gained to be melted slurry and take advantage of heat to pour in mould, in vacuum environment, cool drying 24h under 25 DEG C of conditions, obtained flame retardant rubber;
Step 4, process: get two panels 0.1mm polyurethane film, use methyl alcohol, isopropyl alcohol and acetonitrile mixture ultrasonic degreasing 3 ~ 5min respectively, after clean by washed with de-ionized water, uses acetone wiping, for subsequent use;
Step 5, gluing: temperature be 25 DEG C, relative air humidity is less than in the operating room of 70%, with gasoline by 0.1mm polyurethane film surface clean one time, first dip a small amount of isocyanate glue to wave at gasoline and smear one deck to time half-dried, carry out pregelatinated, then etc. gasoline all volatilize the uniform isocyanate glue of rear painting last layer;
Step 6, glue connect: the polyurethane film of gluing is affixed on flame retardant rubber two sides center position;
Step 7, oven dry: be placed in 40 DEG C of baking ovens and dry 10min.
2. the manufacture method of a kind of flame retardant rubber according to claim 1, is characterized in that, in step 4, in isopropyl alcohol and acetonitrile mixture, the volume ratio of isopropyl alcohol and acetonitrile is 1:1.
3. the manufacture method of a kind of flame retardant rubber according to claim 1, is characterized in that, the 0.1mm polyurethane film in step 4 is the circular membrane of diameter 2cm.
4. the manufacture method of a kind of flame retardant rubber according to claim 1, is characterized in that, in step 5, the thickness of isocyanate glue is 0.08mm thickness.
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| CN104451803A (en) * | 2014-12-22 | 2015-03-25 | 常熟市伟达电镀有限责任公司 | Process for electroplating plastics |
| CN104589773A (en) * | 2014-12-31 | 2015-05-06 | 广西大学 | Method for manufacturing rubber sheet |
| CN104890267A (en) * | 2015-04-25 | 2015-09-09 | 安徽微威胶件集团有限公司 | Rubber sheet production technology |
| CN105799078B (en) * | 2016-03-17 | 2018-08-17 | 青岛科技大学 | It is a kind of to be directly atomized rubber wet method mixing method |
| CN109320804B (en) * | 2018-09-11 | 2021-08-17 | 东莞市雄林新材料科技股份有限公司 | High-hydrolysis-resistance low-voltage variable TPU (thermoplastic polyurethane) film and preparation method thereof |
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| CN1687235A (en) * | 2005-01-31 | 2005-10-26 | 于志斌 | Rubber diaphragm of polyurethane |
| CN101792544A (en) * | 2010-03-30 | 2010-08-04 | 上海工程技术大学 | Environment-friendly flame retardant rubber material and preparation method thereof |
| CN101812193A (en) * | 2009-12-07 | 2010-08-25 | 天津鹏翎胶管股份有限公司 | Formula of environment-friendly flame-retardant chloroprene rubber |
| CN102161787A (en) * | 2011-06-01 | 2011-08-24 | 际华三五三七制鞋有限责任公司 | Environment-friendly flame-retardant rubber for shoe soles and preparation method thereof |
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| JP3336827B2 (en) * | 1995-10-02 | 2002-10-21 | ヤマハ株式会社 | Electronic musical instrument keyboard device |
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|---|---|---|---|---|
| CN1687235A (en) * | 2005-01-31 | 2005-10-26 | 于志斌 | Rubber diaphragm of polyurethane |
| CN101812193A (en) * | 2009-12-07 | 2010-08-25 | 天津鹏翎胶管股份有限公司 | Formula of environment-friendly flame-retardant chloroprene rubber |
| CN101792544A (en) * | 2010-03-30 | 2010-08-04 | 上海工程技术大学 | Environment-friendly flame retardant rubber material and preparation method thereof |
| CN102161787A (en) * | 2011-06-01 | 2011-08-24 | 际华三五三七制鞋有限责任公司 | Environment-friendly flame-retardant rubber for shoe soles and preparation method thereof |
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Effective date of registration: 20170302 Address after: 226400 Rudong City, Jiangsu Province, Yang Kou Chemical Industrial Park Patentee after: Jiangsu Xiangyuan Chemical Co., Ltd. Address before: 215100 Jiangsu, Xiangcheng District Yang Cheng lake town (Hunan City) figure ten Village Patentee before: Suzhou Xiangyuan Speical Fine Chemical Co., Ltd. |