CN102276883A - Production technology for preparing soft condom with grading, low temperature, and long time vulcanization - Google Patents

Production technology for preparing soft condom with grading, low temperature, and long time vulcanization Download PDF

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Publication number
CN102276883A
CN102276883A CN 201110183836 CN201110183836A CN102276883A CN 102276883 A CN102276883 A CN 102276883A CN 201110183836 CN201110183836 CN 201110183836 CN 201110183836 A CN201110183836 A CN 201110183836A CN 102276883 A CN102276883 A CN 102276883A
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China
Prior art keywords
vulcanization
sulphur
stage
zinc oxide
raw materials
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CN 201110183836
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CN102276883B (en
Inventor
张帆
刘翠玲
张宁
秦桂娥
盛冰冰
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QINGDAO DOUBLE BUTTERFLY GROUP CO Ltd
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QINGDAO DOUBLE BUTTERFLY GROUP CO Ltd
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Abstract

The invention relates to a production method of a soft condom, which is a grading, low temperature, and long time vulcanization technology and a vulcanization formula. The production method comprises steps of burdening, a first grade vulcanization, a second stage vulcanization, dipping usage and the like. According to the invention, the consumption of sulfur is reduced to reduce the concentration of a vulcanizing agent, time prolongation and grading vulcanization are used to reach a purpose of a full reaction, an one-time addition of all compounding aids is changed into separated additions of the vulcanizing agent and a vulcanizing activator to prolong the vulcanization time, a two grade vulcanization method and stirring time prolongation are adopted to improve the vulcanization efficiency to completely carry out a crosslinking reaction on the vulcanizing agent, and the latex maturation time prolongation allows properties of a compounding colloid to gradually tend to a stable state and is in favor of subsequent further dipping processing. The transparency and the softness of produced products are obviously improved.

Description

Low temperature vulcanizes the soft condom manufacture technology of preparation for a long time stage by stage
Technical field
The present invention relates to a kind of latex vulcanizate method of producing condom, promptly sulfurizing formula and stage by stage low temperature vulcanize for a long time the preparation soft condom manufacture technology.
Background technology
The natural latex rubber condom is a kind of rubber film goods of making of film forming characteristics that utilize the sulfuration natural rubber latex, be mainly used in preventing property transmission of disease and contraception, along with the domestic and international market demand, the human consumer improves constantly the requirement of condom products, except the safety performance of condom, the human consumer is all to have proposed higher requirement on the flexibility of product and transparency of products and the product odour for product intrinsic quality as the comfortableness of using, comfortable and good feeling is most important concerning the human consumer, and this just needs us to reach requirement by improving prescription and technology.All adopt one time sulfuration process in the existing condom manufacture process, both in the raw latex sulfidation, disposable with whole sulphur etc. all raw materials render in the vulcanizing boiler, the usage quantity of sulphur is big, curing temperature height, time weak point, latex vulcanizate reaction is inhomogeneous, and it is poor to make behind the product transparency and pliability.
Summary of the invention
The purpose of this invention is to provide a kind of vulcanization reaction evenly, few, the transparency of products of sulphur usage quantity and the good sulfuration stage by stage of pliability prepare soft condom manufacture technology.
For achieving the above object, the present invention adopts following technical scheme:
The soft condom manufacture technology of the preparation of sulfuration stage by stage of the present invention is characterized in that comprising the steps:
Low temperature vulcanizes the soft condom manufacture technology of preparation for a long time stage by stage, it is characterized in that comprising the steps:
A) raw material ratio, choose the dry state raw materials in part by weight such as following:
100 parts of sulphur 0.65-0.80 parts, zinc oxide 0.40-0.60 part, zinc dibutyl dithiocarbamate 0.40-0.65 part, 2,6 di tert butyl 4 methyl phenol 0.20-1.00 part, potassium hydroxide 0.10-0.25 part, aliphatic alcohol polyethenoxy (20) ether 0.10-0.30 part, Sodium hexametaphosphate 99 0.10-0.30 part, sodium metnylene bis-naphthalene sulfonate 0.10-0.30 part, raw latex; Respectively aforementioned each dry state raw material is added deionized water and be mixed with the following starting material of mass concentration: natural rubber latex 60%, sulphur 50%, zinc oxide 50%, zinc dibutyl dithiocarbamate 50%, 2,6 di tert butyl 4 methyl phenol 40%, potassium hydroxide 25%, aliphatic alcohol polyethenoxy (20) ether 20%, Sodium hexametaphosphate 99 20%, sodium metnylene bis-naphthalene sulfonate 10%;
B) first stage cure: above-mentioned raw materials in sequence is injected vulcanizing boiler, the usage quantity of sulphur and zinc oxide is 50% of a total amount in this step, the usage quantity of other each compositions is 100%, stirring at normal temperature 30 then---and 60 minutes, in the process of stirring at normal temperature in vulcanizing boiler implantation concentration be that pH value in 10% the ammonia soln adjustment jar is 10.5---11, after finishing, stirring at normal temperature opens the heating controlled temperature at 52-58 ℃, continue to stir and kept 16-20 hour, stop to stir and be cooled to 25 ℃---30 ℃, sealing keeps 5---and 7 days;
C) subordinate phase sulfuration, open the sealing of vulcanizing boiler, start and stir, remaining sulphur dispersion liquid in the steps A proportioning raw materials is injected vulcanizing boiler, remaining zinc oxide fluid dispersion in the proportioning raw materials is injected vulcanizing boiler, stir 30---60 minutes, start heating and temperature is controlled at 45-50 ℃, kept 18-22 hour, be cooled to 25-30 ℃, stop to stir, sealing preserve 24 hours stand-by;
D) dipping uses, and the raw material in the vulcanizing boiler is emitted, and dipping uses behind the accent total solids, does not start stirring during the blowing.
2, the soft condom manufacture technology of the preparation of sulfuration stage by stage according to claim 1, it is characterized in that: in steps A, described dry state raw materials in part by weight is such as following
0.65 part in sulphur, 0.40 part in zinc oxide, 0.40 part of zinc dibutyl dithiocarbamate, 0.20 part of 2,6 di tert butyl 4 methyl phenol, 0.10 part in potassium hydroxide, 0.10 part in aliphatic alcohol polyethenoxy (20) ether, 0.10 part of Sodium hexametaphosphate 99,0.10 part of sodium metnylene bis-naphthalene sulfonate, 100 parts of raw latexs.
3, the soft condom manufacture technology of the preparation of sulfuration stage by stage according to claim 1, it is characterized in that: in steps A, described dry state raw materials in part by weight is such as following
0.70 part in sulphur, 0.50 part in zinc oxide, 0.50 part of zinc dibutyl dithiocarbamate, 0.60 part of 2,6 di tert butyl 4 methyl phenol, 0.15 part in potassium hydroxide, 0.20 part in aliphatic alcohol polyethenoxy (20) ether, 0.20 part of Sodium hexametaphosphate 99,0.20 part of methylene dinaphthalene sulphur, 100 parts of raw latexs.
4, the soft condom manufacture technology of the preparation of sulfuration stage by stage according to claim 1, it is characterized in that: in steps A, described dry state raw materials in part by weight is such as following
0.80 part in sulphur, 0.60 part in zinc oxide, 0.55 part of zinc dibutyl dithiocarbamate, 1.00 parts of 2,6 di tert butyl 4 methyl phenols, 0.25 part in potassium hydroxide, 0.30 part in aliphatic alcohol polyethenoxy (20) ether, 0.30 part of Sodium hexametaphosphate 99,0.30 part of sodium metnylene bis-naphthalene sulfonate, 100 parts of raw latexs.
Technique scheme is in the raw latex sulfidation, and vulcanization reaction is even, and the usage quantity of sulphur reduces, and transparency of products and pliability after making obviously improve.
Embodiment
Embodiment 1:
The soft condom manufacture technology of the preparation of sulfuration stage by stage of the present invention comprises the following steps of carrying out successively:
A) raw material ratio, choose the dry state raw materials in part by weight such as following:
100 parts of sulphur 0.65-0.80 parts, zinc oxide 0.40-0.60 part, zinc dibutyl dithiocarbamate 0.40-0.65 part, 2,6 di tert butyl 4 methyl phenol 0.20-1.00 part, potassium hydroxide 0.10-0.25 part, aliphatic alcohol polyethenoxy (20) ether 0.10-0.30 part, Sodium hexametaphosphate 99 0.10-0.30 part, sodium metnylene bis-naphthalene sulfonate 0.10-0.30 part, raw latex; Respectively aforementioned starting material and deionized water are hybridly prepared into the aqueous solution or emulsion dispersion in water, the shared mass ratio of its mass concentration or solid is respectively: natural rubber latex 60%, sulphur 50%, zinc oxide 50%, zinc dibutyl dithiocarbamate 50%, 2,6-di-tert-butyl-4-methy phenol 40%, potassium hydroxide 25%, aliphatic alcohol polyethenoxy (20) ether 20%, Sodium hexametaphosphate 99 20%, sodium metnylene bis-naphthalene sulfonate 10%
B) first stage cure, be injected in the vulcanizing boiler successively the aqueous solution or the emulsion of above-mentioned raw materials in order, the usage quantity of sulphur and zinc oxide is 50% of a total amount in this step, the usage quantity of other each compositions is 100%, during a kind of dispersion of every adding, carry out towards the rare (PH=7.0 of used deionized water ± 0.5 with deionized water, specific conductivity≤5 μ s/cm :), slowly be filtered in the vulcanizing boiler by 200~300 purpose nets, use the deionized water rinsing charging bucket again, rinse solution is filled in the vulcanizing boiler.Stirring at normal temperature 30 then---and 60 minutes, in the process of stirring at normal temperature in vulcanizing boiler implantation concentration be that pH value in 10% the ammonia soln adjustment jar is 10.5---11, after finishing, stirring at normal temperature opens the heating controlled temperature at 52-58 ℃, continue to stir and kept 16-20 hour, stop stirring and be cooled to 25 ℃---30 ℃.This moment, the sample examination index was: total solids 〉=53%; Viscosity: 15-45mPa.s; Ammonia content: 0.50-0.75%; PH value: 〉=10.5.Sealing keeps 5 then---and 7 days.
C) subordinate phase sulfuration, open the sealing of vulcanizing boiler, start and stir, remaining sulphur dispersion liquid in the steps A proportioning raw materials is injected vulcanizing boiler, remaining zinc oxide fluid dispersion in the proportioning raw materials is injected vulcanizing boiler, stir 30---60 minutes, start heating and temperature is controlled at 45-50 ℃, kept 18-22 hour, measure swelling coefficient 2.2 this moment, be cooled to 25-30 ℃ then, stop to stir.Laboratory indexes should reach total solids 〉=51%, pH value 〉=10.5, swelling coefficient 2.1-2.2 once more, sealing preserve 24 hours stand-by;
D) dipping uses, and the raw material in the vulcanizing boiler is emitted, and dipping uses behind the accent total solids, does not start stirring during the blowing.The processing method of dipping in the use is identical with traditional technology, at this repeated description no longer.
In the present embodiment, vulcanization accelerator is changed into zinc dibutyl dithiocarbamate by zinc diethyldithiocarbamate, the dry state proportioning of sulphur and zinc oxide reduces simultaneously, this is because in traditional sulfidation, be not that all vulcanization aids that add in the latex have all participated in crosslinking reaction, but the vulcanization aid that only enters in the rubber phase has just really participated in crosslinking reaction.Therefore, the purpose that traditional technology heats up is the molecular motion that increases each other, and the frequency of vulcanization aid and latex particle collision is improved, and reaches the purpose of natural rubber latex prevulcanized.And reduce sulfur consumption in the new prescription vulcanizing agent concentration is reduced, by time expand and stage by stage the sulfurized method reach the purpose of abundant reaction, changing into vulcanizing agent and vulcanization leveller by all compounding aids of disposable adding adds at twice and has prolonged curing time and corresponding reduction curing temperature, by vulcanization process stage by stage and prolong churning time and can vulcanize efficient and improve, make the vulcanizing agent crosslinking reaction complete, latex maturation time lengthening can make and cooperate the colloidal property variation progressively to tend towards stability, and is favourable to follow-up further dipping processing.
The product that adopts present embodiment to produce, its explosion and transparency are improved.The tensile property contrast is as follows:
Above-mentioned correlated aging condition: 70 ℃ * 7 days.
The product of present embodiment production can obviously improve tensile yield when keeping tensile strength as can be seen.This product in the proof strength quality, meet under the prerequisite of country and relevant international standard, have good comfort.
Embodiment 2:
With embodiment 1, in steps A, described dry state raw materials in part by weight is such as following
0.70 part in sulphur, 0.50 part in zinc oxide, 0.50 part of zinc dibutyl dithiocarbamate, 0.60 part of 2,6 di tert butyl 4 methyl phenol, 0.15 part in potassium hydroxide, 0.20 part in aliphatic alcohol polyethenoxy (20) ether, 0.20 part of Sodium hexametaphosphate 99,0.20 part of sodium metnylene bis-naphthalene sulfonate, 100 parts of raw latexs.
Embodiment 3:
With embodiment 1, in steps A, described dry state raw materials in part by weight is such as following
0.80 part in sulphur, 0.60 part in zinc oxide, 0.55 part of zinc dibutyl dithiocarbamate, 1.00 parts of 2,6 di tert butyl 4 methyl phenols, 0.25 part in potassium hydroxide, 0.30 part in aliphatic alcohol polyethenoxy (20) ether, 0.30 part of Sodium hexametaphosphate 99,0.30 part of sodium metnylene bis-naphthalene sulfonate, 100 parts of raw latexs.

Claims (4)

1. low temperature vulcanizes the soft condom manufacture technology of preparation for a long time stage by stage, it is characterized in that comprising the steps:
A) raw material ratio, choose the dry state raw materials in part by weight such as following:
100 parts of sulphur 0.65-0.80 parts, zinc oxide 0.40-0.60 part, zinc dibutyl dithiocarbamate 0.40-0.65 part, 2,6 di tert butyl 4 methyl phenol 0.20-1.00 part, potassium hydroxide 0.10-0.25 part, aliphatic alcohol polyethenoxy (20) ether 0.10-0.30 part, Sodium hexametaphosphate 99 0.10-0.30 part, sodium metnylene bis-naphthalene sulfonate 0.10-0.30 part, raw latex; Respectively aforementioned each dry state raw material is added deionized water and be mixed with the following starting material of mass concentration: natural rubber latex 60%, sulphur 50%, zinc oxide 50%, zinc dibutyl dithiocarbamate 50%, 2,6 di tert butyl 4 methyl phenol 40%, potassium hydroxide 25%, aliphatic alcohol polyethenoxy (20) ether 20%, Sodium hexametaphosphate 99 20%, sodium metnylene bis-naphthalene sulfonate 10%;
B) first stage cure: above-mentioned raw materials in sequence is injected vulcanizing boiler, the usage quantity of sulphur and zinc oxide is 50% of a total amount in this step, the usage quantity of other each compositions is 100%, stirring at normal temperature 30 then---and 60 minutes, in the process of stirring at normal temperature in vulcanizing boiler implantation concentration be that pH value in 10% the ammonia soln adjustment jar is 10.5---11, after finishing, stirring at normal temperature opens the heating controlled temperature at 52-58 ℃, continue to stir and kept 16-20 hour, stop to stir and be cooled to 25 ℃---30 ℃, sealing keeps 5---and 7 days;
C) subordinate phase sulfuration, open the sealing of vulcanizing boiler, start and stir, remaining sulphur dispersion liquid in the steps A proportioning raw materials is injected vulcanizing boiler, remaining zinc oxide fluid dispersion in the proportioning raw materials is injected vulcanizing boiler, stir 30---60 minutes, start heating and temperature is controlled at 45-50 ℃, kept 18-22 hour, be cooled to 25-30 ℃, stop to stir, sealing preserve 24 hours stand-by;
D) dipping uses, and the raw material in the vulcanizing boiler is emitted, and dipping uses behind the accent total solids, does not start stirring during the blowing.
2. the soft condom manufacture technology of the preparation of sulfuration stage by stage according to claim 1 is characterized in that: in steps A, described dry state raw materials in part by weight is such as following
0.65 part in sulphur, 0.40 part in zinc oxide, 0.40 part of zinc dibutyl dithiocarbamate, 0.20 part of 2,6 di tert butyl 4 methyl phenol, 0.10 part in potassium hydroxide, 0.10 part in aliphatic alcohol polyethenoxy (20) ether, 0.10 part of Sodium hexametaphosphate 99,0.10 part of sodium metnylene bis-naphthalene sulfonate, 100 parts of raw latexs.
3. the soft condom manufacture technology of the preparation of sulfuration stage by stage according to claim 1 is characterized in that: in steps A, described dry state raw materials in part by weight is such as following
0.70 part in sulphur, 0.50 part in zinc oxide, 0.50 part of zinc dibutyl dithiocarbamate, 0.60 part of 2,6 di tert butyl 4 methyl phenol, 0.15 part in potassium hydroxide, 0.20 part in aliphatic alcohol polyethenoxy (20) ether, 0.20 part of Sodium hexametaphosphate 99,0.20 part of methylene dinaphthalene sulphur, 100 parts of raw latexs.
4. the soft condom manufacture technology of the preparation of sulfuration stage by stage according to claim 1 is characterized in that: in steps A, described dry state raw materials in part by weight is such as following
0.80 part in sulphur, 0.60 part in zinc oxide, 0.55 part of zinc dibutyl dithiocarbamate, 1.00 parts of 2,6 di tert butyl 4 methyl phenols, 0.25 part in potassium hydroxide, 0.30 part in aliphatic alcohol polyethenoxy (20) ether, 0.30 part of Sodium hexametaphosphate 99,0.30 part of sodium metnylene bis-naphthalene sulfonate, 100 parts of raw latexs.
CN2011101838366A 2011-07-01 2011-07-01 Production technology for preparing soft condom under low temperature and long time vulcanization by stages Expired - Fee Related CN102276883B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104479182A (en) * 2014-12-12 2015-04-01 苏州嘉乐威企业发展有限公司 Preparation method of rubber and plastic synthetic ultrathin condom
CN105399997A (en) * 2015-12-31 2016-03-16 上海名邦橡胶制品有限公司 Composition used for preparing latex film product and prevulcanization process thereof
CN107088982A (en) * 2017-04-19 2017-08-25 湖州品创孵化器有限公司 A kind of anti-aging latex seat
CN108504003A (en) * 2018-04-11 2018-09-07 上海正兴阀门制造有限公司 A kind of elastomeric seal loop material and preparation method thereof

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CN101434719A (en) * 2008-12-14 2009-05-20 青岛双蝶集团股份有限公司 Raw material dry state proportion for rubber latex for producing ultrathin condom and formulating vulcanization process thereof
CN101851359A (en) * 2010-06-04 2010-10-06 中国化工橡胶株洲研究设计院 Antibacterial latex prophylactic and production method thereof
CN101891906A (en) * 2010-06-08 2010-11-24 郑林 Nitrosamine-free condom and manufacturing method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1616904A1 (en) * 2004-07-16 2006-01-18 R.T. Vanderbilt Company, Inc. Vulcanizing latex compounds without the use of metal oxide activators or a zinc based accelerator
CN101434719A (en) * 2008-12-14 2009-05-20 青岛双蝶集团股份有限公司 Raw material dry state proportion for rubber latex for producing ultrathin condom and formulating vulcanization process thereof
CN101851359A (en) * 2010-06-04 2010-10-06 中国化工橡胶株洲研究设计院 Antibacterial latex prophylactic and production method thereof
CN101891906A (en) * 2010-06-08 2010-11-24 郑林 Nitrosamine-free condom and manufacturing method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104479182A (en) * 2014-12-12 2015-04-01 苏州嘉乐威企业发展有限公司 Preparation method of rubber and plastic synthetic ultrathin condom
CN105399997A (en) * 2015-12-31 2016-03-16 上海名邦橡胶制品有限公司 Composition used for preparing latex film product and prevulcanization process thereof
CN107088982A (en) * 2017-04-19 2017-08-25 湖州品创孵化器有限公司 A kind of anti-aging latex seat
CN108504003A (en) * 2018-04-11 2018-09-07 上海正兴阀门制造有限公司 A kind of elastomeric seal loop material and preparation method thereof
CN108504003B (en) * 2018-04-11 2020-12-11 上海正兴阀门制造有限公司 Synthetic rubber sealing ring material and preparation method thereof

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