CN109608568A - A kind of Neoprene latex chain rupture technique - Google Patents
A kind of Neoprene latex chain rupture technique Download PDFInfo
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- CN109608568A CN109608568A CN201811459928.0A CN201811459928A CN109608568A CN 109608568 A CN109608568 A CN 109608568A CN 201811459928 A CN201811459928 A CN 201811459928A CN 109608568 A CN109608568 A CN 109608568A
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- 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
- C08F136/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F136/02—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F136/04—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F136/14—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated containing elements other than carbon and hydrogen
- C08F136/16—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated containing elements other than carbon and hydrogen containing halogen
- C08F136/18—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated containing elements other than carbon and hydrogen containing halogen containing chlorine
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Abstract
The present invention relates to neoprene preparation technical fields, specifically disclose a kind of Neoprene latex chain rupture technique, chain-breaker and aqueous slkali is added in the latex that sulphur adjusts when neoprene polymerization reaction terminates, adjust Neoprene latex chain rupture by chain-breaker and aqueous slkali dosage, carried out after chain rupture is qualified subsequent cohesion, it is dry, at rope stripping and slicing, be packaged to be neoprene product.The sulphur adjusting neoprene good product quality that polychloroprene latex Mooney viscosity stability is good, produces, excellent storage stability are adjusted using sulphur after the technical solution chain rupture qualification in this patent.
Description
Technical field
The present invention relates to neoprene preparation technical field, in particular to a kind of Neoprene latex chain rupture technique.
Background technique
Neoprene is divided into sulphur adjustment type and non-sulphur adjustment type, existing sulphur adjustment type neoprene by regulative mode difference
It in process of production, is the Mooney viscosity for reaching product requirement, there are two types of techniques: a kind of in publication number CN107674138A
Described in the Chinese patent of state's patent and publication number CN102040677B, in order to guarantee the good Mooney viscosity stability of product, do not have
There is individual chain rupture technique, but was mutually polymerizeing with addition regulator or chain-breaker, regulator or chain-breaker in water phase oily
Reaction is participated in journey, and qualified polychloroprene latex is obtained after polymerization.It is shown as with the neoprene that this technique produces good
Mooney viscosity stability but product strength deficiency, the bad problem of processing performance.Another technique is traditional handicraft, in alkaline item
Compounds such as dithiocyetetrazole (TETD) are added under part, are broken S -- S, it is viscous to obtain industrial required Mooney
The polymer of degree.Although this traditional handicraft good product quality, chain rupture speed early period is slow, and the decline of later period Mooney viscosity is fast, production
Control is difficult, and product Mooney viscosity stability is poor.
Summary of the invention
The present invention provides a kind of Neoprene latex chain rupture technique, with solve existing two kinds of chain rupture technique production at
Product Mooney viscosity stability is good, but intensity is insufficient；Or product strength foot, but chain rupture speed early period is slow, the decline of later period Mooney viscosity
Fastly, production control is difficult, the problem of product Mooney viscosity stability difference.
In order to achieve the above object, base case of the invention are as follows:
A kind of Neoprene latex chain rupture technique, sulphur adjustment type neoprene polymerization reaction terminate when latex in be added
Chain-breaker and aqueous slkali carry out chain-breaking reaction, and the chain-breaker is the group of Carbamates compound and thiuram compound
It closes.
The technical principle and effect of this base case are:
1, the effect that chain-breaker is added when sulphur adjustment type neoprene polymerization reaction terminates for this base case is: due to
Neoprene polymerization reaction has terminated at this time, therefore is substantially the polymer of macromolecular, these macromolecular polymerics in latex
Object carries out chain rupture under the promotion of chain-breaker, forms polysulfide bond, and polysulfide bond and chlorobutadiene are formed than more complete and uniform poly-
Adduct molecule, so that the product strength of this base case production is high, processing performance is good.In compared to the prior art, in water
Added for chain-breaker in phase, due to being added chain-breaker at this time, macromolecule polyalcohol one formed will by chain-breaker promotion into
And chain rupture generate polysulfide bond, although such technique chain rupture speed is fast, this process be it is indefinite uncontrollable, finally
A large amount of low molecule is usually contained in the polymer of formation, so that the product strength of such technique production is insufficient, processing performance
It is bad.
2, in this base case, when chain-breaker and aqueous slkali are added to sulphur adjusting neoprene polymerization reaction termination simultaneously
Latex in, the thiurams in chain-breaker reacts with aqueous slkali, due to the reaction speed of thiurams and aqueous slkali compared with
Slowly, therefore we in early period joined Carbamates compound, so that chain rupture is quickly carried out, when Carbamates
It closes object to have reacted, since the thiurams in chain breaking process and aqueous slkali meeting sustained response generate Carbamates, energy
Enough guarantee that chain-breaking reaction can continue to carry out, modeling does not occur back, the Mooney viscosity that sulphur adjusts polychloroprene latex after chain rupture is qualified is able to maintain
Stablize, while guaranteeing product quality and product storage stability.
Further, the alkaline solution is NaOH aqueous solution, and the NaOH aqueous solution mass concentration is 3%-6%, control
The amount that NaOH aqueous solution is added, is maintained at the pH value of latex within the scope of 8-12.
The utility model has the advantages that adjusting pH value when chain rupture by the way that NaOH aqueous solution is added when neoprene polymerization reaction terminates
In the range of 8-12, enabling chain-breaking reaction, speed is normally carried out as required, and chain rupture it is qualified after latex Mooney viscosity keep
Relatively stable, the Mooney viscosity of product dodges difference in claimed range.
Further, the parts by weight of the latex are 100, and the parts by weight of the Carbamates compound are X, the value of X
It is less than or equal to 1 greater than 0.
The utility model has the advantages that the addition of Carbamates guarantees there can be faster chain rupture speed early period, chain rupture week is shortened
Phase is verified by testing for several times with production in addition to avoid the excessively multipair rubber quality of Carbamates dosage from having an impact,
In the latex that parts by weight are 100, the parts by weight that Carbamates are added are not greater than 1.
Further, the parts by weight of the thiuram compound are greater than 0 and are less than or equal to 2.
The utility model has the advantages that autumn orchid class chain-breaker can be reacted with alkali, carbaminate is generated, guarantees that chain-breaking reaction can
It is lasting to carry out, it will not occur back to mould phenomenon.Suitable thiuram is neoprene product quality and product storage stability simultaneously
Guarantee, inventor show that the parts by weight of thiuram compound are greater than 0 and are less than or equal in the range of 2 by the verifying tested,
The good product quality that chain rupture obtains.
Further, latex is in the range of temperature during chain-breaking reaction is maintained at 10 DEG C -60 DEG C.
The utility model has the advantages that it is anti-to be normally carried out chain rupture by the latex after the termination of temperature regulating guarantee neoprene polymerization reaction
It answers, returns modeling caused by avoiding reaction speed too fast or later period Mooney viscosity is too low.
Specific embodiment
It is further described below by specific embodiment:
A kind of Neoprene latex chain rupture technique, sulphur adjustment type neoprene polymerization reaction terminate when latex in be added
Chain-breaker and aqueous slkali, chain-breaker are the combination of Carbamates compound and thiuram compound；Wherein chain-breaker can
It to prepare in terminator, or otherwise individually prepares and is added again when polymerization reaction terminates, used in the present embodiment
It individually prepares and is added again when polymerization reaction terminates.
Aqueous slkali is NaOH aqueous solution, and the NaOH aqueous solution that mass concentration is 3-6% is added in the latex of 100g, guarantees
In the range of 8-12, the quality for the Carbamates being in addition added into latex is greater than 0 and is less than or equal to the pH value of latex
1g, the quality of the thiurams of addition are greater than 0 and are less than or equal to 2g, and temperature can be in a specific value in chain breaking process for latex
Fluctuation, the numerical value will be maintained in 10 DEG C -60 DEG C this temperature ranges.
Carbamates compound can select dithiodimethyl carbamic acid sodium, two thiodiethyl carbamic acids
One of sodium or two thio dibutylamino sodium formates, thiuram compound can select two thio tetra methylthiurams,
One of dithiocyetetrazole, two thio tetrabutyl thiurams or two thio four pentyl thiurams.
The following table 1 is the quality and PH that Carbamates compound and thiuram compound are added in embodiment 1-6
It is worth range:
Table 1
Comparative example 1: the Chinese patent of Publication No. CN107674138A discloses a kind of sulphur tune type chlorine of the later period without chain rupture
The preparation method of buna, i.e., after Neoprene latex polymerization, the not no technique of chain rupture, but be added and adjust in water phase
Agent, wherein regulator is two thio dibutylamino sodium formates, and the embodiment for choosing specification [0029] Duan Gongbu is this comparison
Example 1:
The thio dibutylamino sodium formate of 12.5g bis- is added in water phase, prepares sulfur-modified neoprene.It is added in water phase
Emulsifier be rosin.Through detecting, the initial Mooney viscosity average of the sulfur-modified neoprene is 47, and tensile strength is
26.0；Wherein Mooney viscosity is being stood for 24 hours, respectively 43,41 after 36h.
Comparative example 2: for traditional handicraft, i.e., chemical combination such as dithiocyetetrazole (TETD) are added under alkaline condition
Object is broken S -- S, obtains the polymer of industrial required Mooney viscosity.Mooney viscosity 52 after chain rupture is qualified, intensity
29.3；Mooney viscosity is 20 after placing for 24 hours.
Above-described embodiment 1-6 passes through the result that experiment obtains are as follows:
Wherein experiment is using by interval of 0.5-2 hour sampling and testing Mooney viscosities, until chain rupture qualification (Mooney viscosity
It is qualification less than or equal to 65).Re-test Mooney viscosity obtains sulphur tune after chain rupture qualification after chain rupture qualification latex is placed 24 hours
The stability of polychloroprene latex Mooney viscosity.
In addition product quality is examined or check by sulfur modified CR examination criteria and method detection dry glue product, passes through hot-air
Senile experiment, rubber storage stability is examined or check in aging in 70 DEG C of hot air aging casees over three days.
Experimental result is as shown in table 2 below:
Table 2
Conclusion: in conjunction with the experimental data of above-described embodiment 1-6 and the experimental data of comparative example 1-2 it is found that special using this
Sulphur adjusts the sulphur adjusting neoprene that polychloroprene latex Mooney viscosity stability is good, produces after technical solution chain rupture qualification in benefit
Good product quality, excellent storage stability.In short, it is whole to adjust neoprene polymerization reaction in sulphur using technical solution of the present invention
Chain-breaker and aqueous slkali that carbaminate and thiurams are composed are added in latex when only.In chain rupture temperature range
It is interior, Neoprene latex chain rupture is adjusted by adjusting chain-breaker and aqueous slkali dosage, solves that existing there are two types of the Mooneys of technique
Viscosity stability is good, and quality is insufficient or good product quality, but chain rupture speed early period is slow, and the decline of later period Mooney viscosity is fast, production control
System is difficult, the problem of product Mooney viscosity stability difference.The Mooney viscosity that sulphur adjusts polychloroprene latex after chain rupture is qualified is able to maintain surely
It is fixed.High-quality, the product excellent storage stability of sulphur adjusting neoprene product.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (5)
1. a kind of Neoprene latex chain rupture technique, it is characterised in that: when sulphur adjustment type neoprene polymerization reaction terminates
Chain-breaker is added in latex and aqueous slkali carries out chain-breaking reaction, the chain-breaker is Carbamates compound and thiurams
The combination of compound.
2. a kind of Neoprene latex chain rupture technique according to claim 1, it is characterised in that: the aqueous slkali is NaOH
Aqueous solution, the NaOH aqueous solution mass concentration are 3%-6%, and the amount that control NaOH aqueous solution is added protects the pH value of latex
It holds within the scope of 8-12.
3. a kind of Neoprene latex chain rupture technique according to claim 1, it is characterised in that: the parts by weight of the latex
It is 100, the parts by weight of the Carbamates compound are X, and the value of X is greater than 0 and is less than or equal to 1.
4. a kind of Neoprene latex chain rupture technique according to claim 3, it is characterised in that: the thiurams chemical combination
The parts by weight of object are greater than 0 and are less than or equal to 2.
5. a kind of Neoprene latex chain rupture technique according to claim 1 to 4, it is characterised in that: latex is in chain rupture
Temperature is maintained in the range of 10 DEG C -60 DEG C in reaction process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811459928.0A CN109608568B (en) | 2018-11-30 | 2018-11-30 | Chloroprene rubber latex chain breaking process |
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| CN201811459928.0A CN109608568B (en) | 2018-11-30 | 2018-11-30 | Chloroprene rubber latex chain breaking process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669160A (en) * | 2019-10-31 | 2020-01-10 | 重庆化医长寿化工集团有限公司 | Preparation method of neoprene latex for engineering waterproofing |
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|---|---|---|---|---|
| JP2001131234A (en) * | 1999-11-01 | 2001-05-15 | Tosoh Corp | High-elasticity sulfur-modified chloroprene rubber |
| CN1389473A (en) * | 2002-07-16 | 2003-01-08 | 华南理工大学 | Prepn. of powdered neoprene and granulated neoprene |
| CN101284894A (en) * | 2008-06-03 | 2008-10-15 | 重庆长寿化工有限责任公司 | Sulfur-modified neoprene, method for preparing same and applications |
| CN102516618A (en) * | 2011-11-24 | 2012-06-27 | 山西合成橡胶集团有限责任公司 | Compounded emulsion stabilizer in sulfur-modified neoprene rubber |
| CN103554321A (en) * | 2013-09-29 | 2014-02-05 | 安徽同丰橡塑工业有限公司 | Production technology for chloroprene rubber |
| CN104403039A (en) * | 2014-11-07 | 2015-03-11 | 山纳合成橡胶有限责任公司 | Preparation method of sulfur-modified chloroprene rubber with high latex Mooney viscosity stability |
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2018
- 2018-11-30 CN CN201811459928.0A patent/CN109608568B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001131234A (en) * | 1999-11-01 | 2001-05-15 | Tosoh Corp | High-elasticity sulfur-modified chloroprene rubber |
| CN1389473A (en) * | 2002-07-16 | 2003-01-08 | 华南理工大学 | Prepn. of powdered neoprene and granulated neoprene |
| CN101284894A (en) * | 2008-06-03 | 2008-10-15 | 重庆长寿化工有限责任公司 | Sulfur-modified neoprene, method for preparing same and applications |
| CN102516618A (en) * | 2011-11-24 | 2012-06-27 | 山西合成橡胶集团有限责任公司 | Compounded emulsion stabilizer in sulfur-modified neoprene rubber |
| CN103554321A (en) * | 2013-09-29 | 2014-02-05 | 安徽同丰橡塑工业有限公司 | Production technology for chloroprene rubber |
| CN104403039A (en) * | 2014-11-07 | 2015-03-11 | 山纳合成橡胶有限责任公司 | Preparation method of sulfur-modified chloroprene rubber with high latex Mooney viscosity stability |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669160A (en) * | 2019-10-31 | 2020-01-10 | 重庆化医长寿化工集团有限公司 | Preparation method of neoprene latex for engineering waterproofing |
| CN110669160B (en) * | 2019-10-31 | 2022-05-20 | 重庆化医长寿化工集团有限公司 | Preparation method of neoprene latex for engineering water prevention |
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