CN107266724A - A kind of preparation method of hard hollow rubber material - Google Patents

A kind of preparation method of hard hollow rubber material Download PDF

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Publication number
CN107266724A
CN107266724A CN201710608907.XA CN201710608907A CN107266724A CN 107266724 A CN107266724 A CN 107266724A CN 201710608907 A CN201710608907 A CN 201710608907A CN 107266724 A CN107266724 A CN 107266724A
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陈登辉
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00—Compositions of natural rubber
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
    • C08F218/02—Esters of monocarboxylic acids
    • C08F218/04—Vinyl esters
    • C08F218/08—Vinyl acetate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/046—Elimination of a polymeric phase
    • C08J2201/0462—Elimination of a polymeric phase using organic solvents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2307/00—Characterised by the use of natural rubber
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2331/00—Characterised by the use of copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, or carbonic acid, or of a haloformic acid
    • C08J2331/02—Characterised by the use of omopolymers or copolymers of esters of monocarboxylic acids
    • C08J2331/04—Homopolymers or copolymers of vinyl acetate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/18—Spheres
    • C08L2205/20—Hollow spheres

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of preparation method of hard hollow rubber material, the calcium carbonate added in the hollow hard microballoon of the present invention, intensity, the hardness of finished product elastomeric material can effectively be improved, improve the mechanical property of finished-product material, and its light weight, product weight can be reduced, it is readily transported, install, processes, effectively reduce production cost, the hollow hard microballoon of the present invention has good surface organic, the compatibility of each raw material and rubber can be effectively improved, the stability_intensity of finished-product material is improved.

Description

A kind of preparation method of hard hollow rubber material
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of hard hollow rubber material.
Background technology
Natural rubber has the characteristics such as excellent resilience, insulating properties, water-resisting property and plasticity, also, by appropriate place Also there is the valuable property such as oil resistant, acidproof, alkaline-resisting, heat-resisting, cold-resistant, pressure-resistant, wear-resisting after reason, so, with extensive use.For example Rain boots, hot-water bag, the elastic band used in daily life；Surgeon's gloves, blood transfusion tube used in medical and health industry, contraception Set；Conveyer belt, conveyer belt, the acidproof and alkali-resistant gloves industrially used；The irrigation hose that agriculturally uses, ammoniacal liquor bag；It is meteorological Measuring sounding balloon；The sealing of scientific experimentation, shock-absorption；The aircraft that is used in national defence, tank, artillery, gas defence face Tool；The even high-grade, precision and advanced scientific and technical product such as rocket, artificial earth satellite and spaceship all be unable to do without natural rubber；Traffic The various tires used in transport；In order to improve the combination property of rubber, various fillers, Ran Houwu are often added wherein The compatibility of machine filler and rubber is bad, easily causes reunion, reduces the stability of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of system of hard hollow rubber material Preparation Method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of hard hollow rubber material, comprises the following steps：
(1) trimethylolpropane of 1-2 parts by weight is taken, in the absolute ethyl alcohol for being added to 6-8 times of its weight, is stirred；
(2) powdered whiting of 8-10 parts by weight is taken, in the deionized water for being added to 36-40 times of its weight, magnetic agitation 10-16 minutes, mixed with the ethanol solution of above-mentioned trimethylolpropane, rise temperature is 50-60 DEG C, insulated and stirred 1-2 hours, Obtain organic carbonate calcium solution；
(3) methyl methacrylate, the vinylacetate mixing of 10-15 parts by weight of 3-4 parts by weight are taken, reaction is sent to In kettle, rise temperature is 65-70 DEG C, adds the cumyl peroxide of 0.1-0.2 parts by weight, is passed through nitrogen, insulated and stirred 2-3 Hour, obtain polyester liquid；
(4) diethyl that 0.8-1 parts by weight are added under above-mentioned organic carbonate calcium solution, polyester liquid mixing, stirring condition is taken Alkenyl benzene, is sent in ice-water bath, stirring reaction 1-2 hours, discharges, and filtering washes precipitation, air drying, obtains hard and gathers Ester microsphere；
(5) take in the natural rubber powder of 16-20 parts by weight, the tetrahydrofuran for being added to 6-10 times of its weight, stir；
(6) above-mentioned hard polyester microballoon is taken, mixes, stirs with the tetrahydrofuran solution of rubber powder, rise temperature is 50-60 DEG C, the 2-mercaptobenzimidazole of 0.5-1 parts by weight is added, is distilled off at tetrahydrofuran, 90-95 DEG C of vacuum drying 1-2 Hour, obtain hard polyester latex microspheres；
(7) take in above-mentioned hard oligomer rubber powder microballoon, the acetone soln for being added to 10-13 times of its weight, in 60-70 Insulated and stirred 2-3 hours at DEG C, filtering washs precipitation with acetone, deionized water successively, and 1-2 is dried at 110-120 DEG C of vacuum Hour, hard-hearted matter rubber powder of having leisure；
(8) above-mentioned hollow vulcanie powder is taken, natural rubber, the age resistor of 2-3 parts by weight with 100-120 parts by weight 688th, the polybenzimidazoles mixing of 0.6-1 parts by weight, is sent in banbury, banburying 30-40s, and mixing temperature is 60-100 DEG C, The tricaprylate of triethylene glycol two, the inositol of 2-4 parts by weight of 6-9 parts by weight are added, is kneaded 6-8 minutes, dumping is cooled to 10-40 DEG C, put into mill, add the sulphur of accelerator TL, 0.8-1 parts by weight of 1-2 parts by weight, it is thin logical 3-5 times, produce The hard hollow rubber material.
Advantages of the present invention：
The present invention is first handled powdered whiting by the ethanol solution of trimethylolpropane, obtains organic carbonate calcium molten Liquid, then using vinylacetate, methyl methacrylate as monomer, cumyl peroxide is initiator, is polymerize, and is obtained Polyester liquid, then mixes it with organic carbonate calcium solution, by divinyl benzene crosslinked, obtains calcium carbonate cross-linked polyester micro- Ball, then the tetrahydrofuran solution with natural rubber powder mix, obtain hard polyester latex microspheres, be then dispersed in acetone In, polyvinyl acetate is dissolved, hollow hard microballoon is obtained；
The calcium carbonate that adds in the hollow hard microballoon of the present invention, can effectively improve finished product elastomeric material intensity, Hardness, improves the mechanical property of finished-product material, and its light weight, can reduce product weight, be readily transported, install, process, effectively Reduction production cost, hollow hard microballoon of the invention has good surface organic, can effectively improve each raw material With the compatibility of rubber, the stability_intensity of finished-product material is improved.
Embodiment
Embodiment 1
A kind of preparation method of hard hollow rubber material, comprises the following steps：
(1) trimethylolpropane of 2 parts by weight is taken, in the absolute ethyl alcohol for being added to 8 times of its weight, is stirred；
(2) powdered whiting of 10 parts by weight is taken, in the deionized water for being added to 40 times of its weight, 16 points of magnetic agitation Clock, is mixed with the ethanol solution of above-mentioned trimethylolpropane, and rise temperature is 60 DEG C, and insulated and stirred 2 hours obtains organic carbonate calcium Solution；
(3) methyl methacrylate, the vinylacetate mixing of 15 parts by weight of 4 parts by weight are taken, is sent in reactor, It is 70 DEG C to raise temperature, adds the cumyl peroxide of 0.2 parts by weight, is passed through nitrogen, insulated and stirred 3 hours obtains polyester molten Liquid；
(4) divinyl that 1 parts by weight are added under above-mentioned organic carbonate calcium solution, polyester liquid mixing, stirring condition is taken Benzene, is sent in ice-water bath, stirring reaction 2 hours, discharges, and precipitation is washed in filtering, and air drying obtains hard polyester microballoon；
(5) the natural rubber powder of 20 parts by weight is taken, in the tetrahydrofuran for being added to 10 times of its weight, is stirred；
(6) above-mentioned hard polyester microballoon is taken, mixes, stirs with the tetrahydrofuran solution of rubber powder, rise temperature is 60 DEG C, the 2-mercaptobenzimidazole of 1 parts by weight is added, is distilled off drying 2 hours at tetrahydrofuran, 95 DEG C of vacuum, obtains hard Lactoprene microballoon；
(7) take in above-mentioned hard oligomer rubber powder microballoon, the acetone soln for being added to 13 times of its weight, protected at 70 DEG C Temperature stirring 3 hours, filtering washs precipitation with acetone, deionized water successively, is dried 2 hours at 120 DEG C of vacuum, has leisure hard-hearted Matter rubber powder；
(8) above-mentioned hollow vulcanie powder is taken, age resistor 688, the 0.6- of natural rubber, 3 parts by weight with 120 parts by weight The polybenzimidazoles mixing of 1 parts by weight, is sent in banbury, banburying 40s, and mixing temperature is 60-100 DEG C, adds 6-9 weight The tricaprylate of triethylene glycol two, the inositol of 4 parts by weight of part, are kneaded 8 minutes, dumping, are cooled to 40 DEG C, put into mill It is interior, accelerator TL, the sulphur of 1 parts by weight of 2 parts by weight are added, it is thin logical 5 times, produce the hard hollow rubber material.
Embodiment 2
(1) trimethylolpropane of 1 parts by weight is taken, in the absolute ethyl alcohol for being added to 6 times of its weight, is stirred；
(2) powdered whiting of 8 parts by weight is taken, in the deionized water for being added to 36 times of its weight, magnetic agitation 10 minutes, Mixed with the ethanol solution of above-mentioned trimethylolpropane, rise temperature is 50 DEG C, and insulated and stirred 1 hour obtains organic carbonate calcium molten Liquid；
(3) methyl methacrylate, the vinylacetate mixing of 10 parts by weight of 3 parts by weight are taken, is sent in reactor, It is 65 DEG C to raise temperature, adds the cumyl peroxide of 0.1 parts by weight, is passed through nitrogen, insulated and stirred 2 hours obtains polyester molten Liquid；
(4) divinyl that 0.8 parts by weight are added under above-mentioned organic carbonate calcium solution, polyester liquid mixing, stirring condition is taken Base benzene, is sent in ice-water bath, stirring reaction 1 hour, discharges, and precipitation is washed in filtering, and air drying obtains hard polyester micro- Ball；
(5) the natural rubber powder of 16 parts by weight is taken, in the tetrahydrofuran for being added to 6 times of its weight, is stirred；
(6) above-mentioned hard polyester microballoon is taken, mixes, stirs with the tetrahydrofuran solution of rubber powder, rise temperature is 50 DEG C, the 2-mercaptobenzimidazole of 0.5 parts by weight is added, is distilled off drying 1 hour at tetrahydrofuran, 90 DEG C of vacuum, obtains firmly Matter lactoprene microballoon；
(7) take in above-mentioned hard oligomer rubber powder microballoon, the acetone soln for being added to 10 times of its weight, protected at 60 DEG C Temperature stirring 2 hours, filtering washs precipitation with acetone, deionized water successively, is dried 1 hour at 110 DEG C of vacuum, has leisure hard-hearted Matter rubber powder；
(8) above-mentioned hollow vulcanie powder is taken, the age resistor 688,0.6 of natural rubber, 2 parts by weight with 100 parts by weight The polybenzimidazoles mixing of parts by weight, is sent in banbury, banburying 30s, and mixing temperature is 60 DEG C, adds the three of 6 parts by weight The tricaprylate of ethylene glycol two, the inositol of 2 parts by weight, are kneaded 6 minutes, dumping, are cooled in 10 DEG C, input mill, plus Enter accelerator TL, the sulphur of 0.8 parts by weight of 1 parts by weight, it is thin logical 3 times, produce the hard hollow rubber material.
Performance test：
The material of the present invention：
Stretch breaking strength (MPa)：17-21；
Surely modulus 100% (MPa) is stretched：2.4-2.8；
70 DEG C × 70h air oven aging tests：
Breaking strength reduced rate：4-4.5%, elongation at break reduced rate：7.6-8%；
Traditional natural rubber material：
Stretch breaking strength (MPa)：10-13；
Surely modulus 100% (MPa) is stretched：1.7-2；
70 DEG C × 70h air oven aging tests：
Breaking strength reduced rate：7-9%, elongation at break reduced rate：13-19%.

Claims (1)

1. a kind of preparation method of hard hollow rubber material, it is characterised in that comprise the following steps：
(1) trimethylolpropane of 1-2 parts by weight is taken, in the absolute ethyl alcohol for being added to 6-8 times of its weight, is stirred；
(2) powdered whiting of 8-10 parts by weight is taken, in the deionized water for being added to 36-40 times of its weight, magnetic agitation 10-16 Minute, mixed with the ethanol solution of above-mentioned trimethylolpropane, rise temperature is 50-60 DEG C, and insulated and stirred 1-2 hours must have Machine calcium carbonate soln；
(3) methyl methacrylate, the vinylacetate mixing of 10-15 parts by weight of 3-4 parts by weight are taken, reactor is sent to In, rise temperature is 65-70 DEG C, adds the cumyl peroxide of 0.1-0.2 parts by weight, is passed through nitrogen, insulated and stirred 2-3 is small When, obtain polyester liquid；
(4) divinyl that 0.8-1 parts by weight are added under above-mentioned organic carbonate calcium solution, polyester liquid mixing, stirring condition is taken Benzene, is sent in ice-water bath, stirring reaction 1-2 hours, discharges, and precipitation is washed in filtering, and air drying obtains hard polyester micro- Ball；
(5) take in the natural rubber powder of 16-20 parts by weight, the tetrahydrofuran for being added to 6-10 times of its weight, stir；
(6) above-mentioned hard polyester microballoon is taken, mixes, stirs with the tetrahydrofuran solution of rubber powder, rise temperature is 50-60 DEG C, the 2-mercaptobenzimidazole of 0.5-1 parts by weight is added, is distilled off drying 1-2 hours at tetrahydrofuran, 90-95 DEG C of vacuum, Obtain hard polyester latex microspheres；
(7) take in above-mentioned hard oligomer rubber powder microballoon, the acetone soln for being added to 10-13 times of its weight, at 60-70 DEG C Insulated and stirred 2-3 hours, filtering, precipitation is washed successively with acetone, deionized water, 1-2 is dried at 110-120 DEG C of vacuum small When, hard-hearted matter rubber powder of having leisure；
(8) above-mentioned hollow vulcanie powder is taken, the age resistor 688 of natural rubber, 2-3 parts by weight with 100-120 parts by weight, The polybenzimidazoles mixing of 0.6-1 parts by weight, is sent in banbury, banburying 30-40s, and mixing temperature is 60-100 DEG C, is added The tricaprylate of triethylene glycol two, the inositol of 2-4 parts by weight of 6-9 parts by weight, are kneaded 6-8 minutes, dumping is cooled to 10- 40 DEG C, put into mill, add the sulphur of accelerator TL, 0.8-1 parts by weight of 1-2 parts by weight, it is thin logical 3-5 times, produce institute State hard hollow rubber material.
CN201710608907.XA 2017-07-24 2017-07-24 A kind of preparation method of hard hollow rubber material Pending CN107266724A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108192172A (en) * 2017-12-07 2018-06-22 厉展源 A kind of preparation method of vulcanie
CN108484997A (en) * 2018-04-27 2018-09-04 中国科学院青岛生物能源与过程研究所 Hollow polystyrene microsphere enhancing composite natral rubber material of a kind of single port and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1528815A (en) * 2003-09-29 2004-09-15 华南理工大学 In situ modified waste rubber powder composite material and preparing method thereof
CN103450516A (en) * 2013-08-02 2013-12-18 山东永泰化工集团有限公司 Rubber tire tread and milling process thereof
CN103483656A (en) * 2013-09-22 2014-01-01 苏州市湘园特种精细化工有限公司 Reprocessing method for waste rubber
CN104387641A (en) * 2014-12-17 2015-03-04 江西省万载橡塑有限公司 Modified rubber powder and preparation method thereof
CN105001569A (en) * 2015-07-07 2015-10-28 四川大学 Polyvinyl alcohol/shell powder biomass composite material and preparation method therefor
CN105461981A (en) * 2015-12-17 2016-04-06 合肥杰明新材料科技有限公司 Oxidization-resistant natural rubber material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1528815A (en) * 2003-09-29 2004-09-15 华南理工大学 In situ modified waste rubber powder composite material and preparing method thereof
CN103450516A (en) * 2013-08-02 2013-12-18 山东永泰化工集团有限公司 Rubber tire tread and milling process thereof
CN103483656A (en) * 2013-09-22 2014-01-01 苏州市湘园特种精细化工有限公司 Reprocessing method for waste rubber
CN104387641A (en) * 2014-12-17 2015-03-04 江西省万载橡塑有限公司 Modified rubber powder and preparation method thereof
CN105001569A (en) * 2015-07-07 2015-10-28 四川大学 Polyvinyl alcohol/shell powder biomass composite material and preparation method therefor
CN105461981A (en) * 2015-12-17 2016-04-06 合肥杰明新材料科技有限公司 Oxidization-resistant natural rubber material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108192172A (en) * 2017-12-07 2018-06-22 厉展源 A kind of preparation method of vulcanie
CN108484997A (en) * 2018-04-27 2018-09-04 中国科学院青岛生物能源与过程研究所 Hollow polystyrene microsphere enhancing composite natral rubber material of a kind of single port and preparation method thereof

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Application publication date: 20171020