CN103483657A - Reprocessing method for flame retardant rubber - Google Patents
Reprocessing method for flame retardant rubber Download PDFInfo
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- CN103483657A CN103483657A CN201310430862.3A CN201310430862A CN103483657A CN 103483657 A CN103483657 A CN 103483657A CN 201310430862 A CN201310430862 A CN 201310430862A CN 103483657 A CN103483657 A CN 103483657A
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Abstract
The invention belongs to the field of machinery manufacture, and particularly relates to a reprocessing method for flame retardant rubber. The method comprises the following steps: waste rubber is treated through the seven steps of grinding, cleaning, melting, modifying, vacuum defoamation, sizing and vulcanization, an oxygen plasma active carbon tube, modified starch and pigment are added, and are mixed uniformly together with rubber cement for modification, wherein the content of the oxygen plasma active carbon tube is 1-5%, and the content of the modified starch is 3-8%. Through a series of treatment to waste rubber, not only is the purpose of turning waste into wealth realized, but also the old rubber is purified, the high ductility, oxidation resistance and flame resistance of the reproduced rubber are enhanced.
Description
Technical field
The invention belongs to mechanical manufacturing field, be specifically related to a kind of process for subsequent treatment of flame retardant rubber.
Background technology
Rubber is common industrial production wheel, travelling belt, construct the essential product of object, the consumption in rubber every year is also very surprising, how to deal carefully with waste rubber and become urgent problem, turning waste into wealth is the main stream approach of rubberized, the process for subsequent treatment of waste rubber also becomes very important so, irrational reprocessing can not meet the condition of the share while wasting manpower and material resources of rubber most probably, the present invention proposes a kind of process for subsequent treatment of flame retardant rubber, the both old rubber of regeneration activating, also give regeneration and produce some character that originally do not have of rubber simultaneously, extend rubber work-ing life, also improved security.
Summary of the invention
For the deficiency existed on prior art, the invention provides a kind of process for subsequent treatment of waste rubber of turning waste into wealth.
To achieve these goals, the present invention realizes by the following technical solutions:
1. the process for subsequent treatment of a flame retardant rubber, is characterized in that,
1) pulverize: waste Crumb rubber is broken into to 100～300 purpose rubber powders;
2) clean: by rubber powder respectively successively with mixture, acetone and the deionized water of ethanol and ether respectively in industrial ultrasonic machine ultrasound filtration clean half hour, more sequentially clean three times with 93# gasoline and deionized water;
3) melt: the rubber powder that will clean is put into reactor, and 300 ℃, heat 30min under agitation condition, make it become melting rubber cement state;
4) modification: add oxygen plasma activated carbon pipe, treated starch and pigment in reactor, stir with rubber cement; The content of described oxygen plasma activated carbon pipe is 1%～5%, and the content of described treated starch is 3%～8%;
5) vacuum defoamation: reactor is evacuated, takes the air dissolved in rubber cement away, slough the bubble in rubber cement;
6) typing: emit rubber cement from reactor to mould, vacuum cooling 3～4h, when rubber cement becomes half-dried, sprinkle the nano flame retardant mixture, more cooling 3～4h, to complete drying;
The preparation method of described described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, 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 mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, dry 24 hours of 60 ℃ of temperature, grinding is sieved, and obtains the modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.Filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at the 600W power ultrasonic, be heated to 90 ℃ with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain the nano flame retardant mixture;
7) sulfuration: use sulphur and calcium carbonate to carry out at 130～140 ℃, under pressure 15MPa condition, vulcanize 30min, pass into hydrogen sulfide in sulfidation, help sulfuration fully.
In the process for subsequent treatment of above-mentioned waste rubber, described step 2) in, in the mixture of described ethanol and ether, ethanol: ether=5:2.
In the process for subsequent treatment of above-mentioned waste rubber, described step 4), described oxygen plasma activated carbon pipe treatment condition are under the vacuum stirring condition, the logical oxygen 1h of high temperature processes the carbon pipe.
In the process for subsequent treatment of above-mentioned waste rubber, described step 4) in, described treated starch is cross-linking starch.
Beneficial effect: the waste rubber process is pulverized, clean, melt, modification, vacuum defoamation, the typing and vulcanize the processing of seven steps after, not only turn waste into wealth, and by after a series of processing to waste rubber, purify old rubber, increase regeneration and produce the ductility of rubber, oxidation-resistance and flame retardant resistance, pulverize the rubber powder particle diameter suitable, without using meticulous instrument, processed, water-soluble and the lipid-soluble substance on scrap rubber surface is removed in cleaning, improve the scrap rubber quality, in modification, oxygen plasma activated carbon pipe improves resistance of aging, increase the service life, treated starch add increase ductility, be in harmonious proportion the adding of pigment the ugly color of scrap rubber, give the visual sense of security of client, vacuum defoamation increases rubber compactness, when rubber cement becomes half-dried, mixture is adsorbed in to rubber surface, play fire-retardant effect.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, have a extensive future; The present invention carries out twice-modified, such benefit: increase the reactive behavior point, improve modified effect; In the time of modification, can steam again except the moisture in system, dry and modification is carried out simultaneously, has improved working efficiency; Have a large amount of physics and chemistry planar water in nano silicone hydroxyapatite, Attapulgite, polynite, kaolin etc. self micropore, at high temperature produce water vapor, blocking-up oxygen, absorb heat, reaches multiple fire-retardant effect; Powerful absorption property can effectively improve the synergy of several fire retardants, stops and is raise by the fire retardant matter temperature, has improved flame retarding efficiency; The aboundresources such as silicon hydroxyapatite, Attapulgite, polynite, kaolin, greatly reduce the industrial cost of fire retardant, and also the Application and Development for attapulgite provides a new way; The present invention adopts the solution method ultrasonic wave to disperse and the mechanical high-speed agitator stirs, make fire retardant separately component reached the nano level dispersion in solution, effectively avoided the natural oxidation to matrix material, thereby made matrix material there is better mechanical property.The oxygen index of matrix material is 39.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
Embodiment 1:
2. the process for subsequent treatment of a flame retardant rubber, is characterized in that,
1) pulverize: waste Crumb rubber is broken into to 100～300 purpose rubber powders;
2) clean: by rubber powder respectively successively with mixture, acetone and the deionized water of ethanol and ether respectively in industrial ultrasonic machine ultrasound filtration clean half hour, more sequentially clean three times with 93# gasoline and deionized water;
3) melt: the rubber powder that will clean is put into reactor, and 300 ℃, heat 30min under agitation condition, make it become melting rubber cement state;
4) modification: add oxygen plasma activated carbon pipe, treated starch and pigment in reactor, stir with rubber cement; The content of described oxygen plasma activated carbon pipe is 1%～5%, and the content of described treated starch is 3%～8%;
5) vacuum defoamation: reactor is evacuated, takes the air dissolved in rubber cement away, slough the bubble in rubber cement;
6) typing: emit rubber cement from reactor to mould, vacuum cooling 3～4h, when rubber cement becomes half-dried, sprinkle the nano flame retardant mixture, more cooling 3～4h, to complete drying;
The preparation method of described described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, 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 mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, dry 24 hours of 60 ℃ of temperature, grinding is sieved, and obtains the modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.Filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at the 600W power ultrasonic, be heated to 90 ℃ with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain the nano flame retardant mixture;
7) sulfuration: use sulphur and calcium carbonate to carry out at 130～140 ℃, under pressure 15MPa condition, vulcanize 30min, pass into hydrogen sulfide in sulfidation, help sulfuration fully.
Wherein, in the mixture of described ethanol and ether, ethanol: ether=5:2.
Crucial, described oxygen plasma activated carbon pipe treatment condition are under the vacuum stirring condition, and the logical oxygen 1h of high temperature processes the carbon pipe, and described treated starch is cross-linking starch.
And, in the mixture of described magnesium aluminum-hydrotalcite, ammonium polyphosphate and magnesium hydroxide, the ratio of magnesium aluminum-hydrotalcite, ammonium polyphosphate and magnesium hydroxide is 2:1:2.
In the present embodiment, select suitable oxygen plasma activated carbon pipe and treated starch content in modification procedure, ductility, than not adding or few 2 times of fashions that add, detects and obtains 1 times of ageing resistance raising by accelerated test.
Embodiment 2: all the other are identical with described embodiment 1, difference is, first vacuum cooling 4h in step 6), cooling 4h again, in the present embodiment, the rubber flame-retarded effect of gained is slightly poorer than embodiment 1, but the mixture consumption of magnesium aluminum-hydrotalcite, ammonium polyphosphate and magnesium hydroxide is low, does not affect result of use.
Embodiment 3: all the other are identical with described embodiment 1, and difference is, changes cure conditions in step 7): 140 ℃, under pressure 15MPa condition, vulcanize 30min.
The present invention is applicable to other Retreatment methods of waste old, as 4) time only add treated starch or oxygen plasma activated carbon pipe, 6) time do not add mixture of magnesium aluminum-hydrotalcite, ammonium polyphosphate and magnesium hydroxide etc.
The present embodiment is known in practical application, the present invention pulverizes the waste rubber process, clean, melt, modification, vacuum defoamation, the typing and vulcanize the processing of seven steps after, not only turn waste into wealth, and by after a series of processing to waste rubber, purify old rubber, increase regeneration and produce the ductility of rubber, oxidation-resistance and flame retardant resistance, pulverize the rubber powder particle diameter suitable, without using meticulous instrument, processed, water-soluble and the lipid-soluble substance on scrap rubber surface is removed in cleaning, improve the scrap rubber quality, in modification, oxygen plasma activated carbon pipe improves resistance of aging, increase the service life, treated starch add increase ductility, be in harmonious proportion the adding of pigment the ugly color of scrap rubber, give the visual sense of security of client, vacuum defoamation increases rubber compactness, when rubber cement becomes half-dried, mixture is adsorbed in to rubber surface, play fire-retardant effect.
Above demonstration and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. the process for subsequent treatment of a flame retardant rubber, is characterized in that,
1) pulverize: waste Crumb rubber is broken into to 100～300 purpose rubber powders;
2) clean: by rubber powder respectively successively with mixture, acetone and the deionized water of ethanol and ether respectively in industrial ultrasonic machine ultrasound filtration clean half hour, more sequentially clean three times with 93# gasoline and deionized water;
3) melt: the rubber powder that will clean is put into reactor, and 300 ℃, heat 30min under agitation condition, make it become melting rubber cement state;
4) modification: add oxygen plasma activated carbon pipe, treated starch and pigment in reactor, stir with rubber cement; The content of described oxygen plasma activated carbon pipe is 1%～5%, and the content of described treated starch is 3%～8%;
5) vacuum defoamation: reactor is evacuated, takes the air dissolved in rubber cement away, slough the bubble in rubber cement;
6) typing: emit rubber cement from reactor to mould, vacuum cooling 3～4h, when rubber cement becomes half-dried, sprinkle the nano flame retardant mixture, more cooling 3～4h, to complete drying;
The preparation method of described described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, 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 mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, dry 24 hours of 60 ℃ of temperature, grinding is sieved, and obtains the modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.
2. filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at the 600W power ultrasonic, be heated to 90 ℃ with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain the nano flame retardant mixture;
7) sulfuration: use sulphur and calcium carbonate to carry out at 130～140 ℃, under pressure 15MPa condition, vulcanize 30min, pass into hydrogen sulfide in sulfidation, help sulfuration fully.
3. the process for subsequent treatment of waste rubber according to claim 1, is characterized in that, described step 2) in, in the mixture of described ethanol and ether, ethanol: ether=5:2.
4. the process for subsequent treatment of waste rubber according to claim 1, is characterized in that, described step 4), described oxygen plasma activated carbon pipe treatment condition are under the vacuum stirring condition, the logical oxygen 1h of high temperature processes the carbon pipe.
5. the process for subsequent treatment of waste rubber according to claim 1, is characterized in that, described step 4) in, described treated starch is cross-linking starch.
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| CN201310430862.3A CN103483657B (en) | 2013-09-22 | 2013-09-22 | Reprocessing method for flame retardant rubber |
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| CN201310430862.3A CN103483657B (en) | 2013-09-22 | 2013-09-22 | Reprocessing method for flame retardant rubber |
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| CN103483657B CN103483657B (en) | 2015-05-20 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804312A (en) * | 2015-04-27 | 2015-07-29 | 安徽美祥实业有限公司 | Rubber production process |
| CN104893057A (en) * | 2015-06-08 | 2015-09-09 | 苏州市湘园特种精细化工有限公司 | Reprocessing method of waste rubber |
| CN105670069A (en) * | 2016-01-13 | 2016-06-15 | 浙江世泰实业有限公司 | Manufacturing process of hydraulic mount's rubber main spring |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101418104A (en) * | 2008-10-27 | 2009-04-29 | 江苏省国祥塑胶有限公司 | Waste polyvinyl chloride and waste rubber blending system and preparation method |
| CN101974173A (en) * | 2010-10-18 | 2011-02-16 | 江汉大学 | Microwave activated waste rubber powder-containing flame retardant rubber plate and preparation method thereof |
| WO2011113148A1 (en) * | 2010-03-15 | 2011-09-22 | 4463251 Canada Inc. | Method and apparatus for regenerating vulcanized rubber |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101418104A (en) * | 2008-10-27 | 2009-04-29 | 江苏省国祥塑胶有限公司 | Waste polyvinyl chloride and waste rubber blending system and preparation method |
| WO2011113148A1 (en) * | 2010-03-15 | 2011-09-22 | 4463251 Canada Inc. | Method and apparatus for regenerating vulcanized rubber |
| CN101974173A (en) * | 2010-10-18 | 2011-02-16 | 江汉大学 | Microwave activated waste rubber powder-containing flame retardant rubber plate and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804312A (en) * | 2015-04-27 | 2015-07-29 | 安徽美祥实业有限公司 | Rubber production process |
| CN104893057A (en) * | 2015-06-08 | 2015-09-09 | 苏州市湘园特种精细化工有限公司 | Reprocessing method of waste rubber |
| CN105670069A (en) * | 2016-01-13 | 2016-06-15 | 浙江世泰实业有限公司 | Manufacturing process of hydraulic mount's rubber main spring |
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