CN103570875A - Preparation method of chloroprene rubber - Google Patents

Preparation method of chloroprene rubber Download PDF

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CN103570875A
CN103570875A CN201310546658.8A CN201310546658A CN103570875A CN 103570875 A CN103570875 A CN 103570875A CN 201310546658 A CN201310546658 A CN 201310546658A CN 103570875 A CN103570875 A CN 103570875A
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weight
weight part
preparation
oil phase
solution
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张成如
刘霞
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Jinan Development Zone Xinghuo Technology Research Institute
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Jinan Development Zone Xinghuo Technology Research Institute
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Abstract

The invention belongs to the technical field of production of chloroprene rubbers, and in particular relates to a preparation method of a chloroprene rubber. The preparation method of the chloroprene rubber comprises the steps of (1) preparation; (2) polymerization; (3) termination and chain rupture; (4) agglomeration and drying. The preparation method is simple in step and easy to operate, the electrical insulation property and cold resistance of the obtained chloroprene rubber are greatly improved, and the stability during storage is greatly enhanced at the same time.

Description

A kind of preparation method of chloroprene rubber
Technical field
The invention belongs to the technical field that chloroprene rubber is produced, be specifically related to a kind of preparation method of chloroprene rubber.
Background technology
Chloroprene rubber is to take chloroprene as main raw material, by homopolymerization or on a small quantity other monomer copolymerization form.The tensile strength of chloroprene rubber is high, its rubber item heat-resisting, fast light, ageing-resistant performance is good, oil resistance is all better than natural rubber, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber.Have stronger flame resistivity and excellent fire retardance, its chemical stability is higher, and water tolerance is good.The shortcoming of chloroprene rubber is electrical insulation capability, and cold tolerance is poor, and rubber is unstable when storing.
Chloroprene rubber is of many uses, can be applied to different technical fields, is mainly used in rubber industry field, makes travelling belt and transmission belt as being used for, and the foreskin material of electric wire, cable is manufactured the equipment lining of oil resisting rubber hose, packing ring and resistance to chemical attack.Simultaneously also very extensive in the application in elastomerics field, for example dipped goods is as played an important role in gloves, extruded foam material, asphalt modification.
Rubber industry is one of important foundation industry of national economy.It not only provides daily life the indispensable light industry rubber product such as daily, medical for people, and provides various rubber production unit processed or rubber components to the heavy industry such as digging, traffic, building, machinery, electronics and new industry.Visible, the product category of rubber industry is various, and backward industry is very wide.
Summary of the invention
The object of the invention is to for the defect of above-mentioned existence and a kind of preparation method of chloroprene rubber is provided, the method step is simple, processing ease, resulting chloroprene rubber electrical insulation capability, the getable improvement greatly of winter hardiness are strengthened in stable upon storage performance simultaneously greatly.
Technical scheme of the present invention is: a kind of preparation method of chloroprene rubber, comprises the following steps:
(1) preparation: the chloroprene drying of 100~120 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.6~0.8 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 3.5~4.5 weight parts completely, and preparation obtains oil phase; The dispersion agent of 130~150 weight part softening waters, 0.65~0.75 weight part sodium hydroxide, 0.85~0.95 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 0.2~1.0 weight part, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution;
(2) polymerization: by oil phase and water by weight 1:(1~2) be placed in emulsifying kettle at 20~25 ℃ after mixing and emulsifying, deliver to polymeric kettle, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is (0.2~0.35): 1; Then at 40~45 ℃, carry out polyreaction 2~2.5 hours, obtain latex;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is (0.15~0.3): 1; Then latex is placed in and in chain rupture groove, carries out alkaline chain rupture;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product.
The preparation method of described chloroprene rubber, comprises the following steps:
(1) preparation: the chloroprene drying of 115 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.75 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 4 weight parts completely, and preparation obtains oil phase; The dispersion agent of 145 weight part softening waters, 0.7 weight part sodium hydroxide, 0.9 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 0.25 weight part, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution;
(2) polymerization: oil phase and water are placed in emulsifying kettle and after mixing and emulsifying, deliver to polymeric kettle at 23 ℃ by weight 1:1.5, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is 0.3:1; Then at 42 ℃, carry out polyreaction 2.5 hours, obtain latex;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is 0.25:1; Then latex is placed in and in chain rupture groove, carries out alkaline chain rupture;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product.
The 1-chloro-1,3-butadiene that the chlorbutadiene that chloroprene in described step (1) is 96.5% by weight fraction and weight fraction are 3.5%.
In described step (3), in latex relative density, reach at 1.068 o'clock and add terminator solution.
In described step (4), flocculation agent is comprised of the sodium-chlor of 0.55 weight part and the calcium chloride of 0.65 weight part.
Beneficial effect of the present invention is: the preparation method of chloroprene rubber of the present invention, and step is simple, processing ease, resulting chloroprene rubber electrical insulation capability, cold tolerance have obtained improving greatly, in stable upon storage performance, greatly strengthen simultaneously.
Embodiment
Below by specific embodiment, the present invention will be described in detail.
Embodiment 1
A preparation method for chloroprene rubber, comprises the following steps:
(1) preparation: the chloroprene drying of 100 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.6 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 3.5 weight parts completely, and preparation obtains oil phase; The dispersion agent of 130 weight part softening waters, 0.65 weight part sodium hydroxide, 0.85 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 0.2 weight part, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution; The 1-chloro-1,3-butadiene that the chlorbutadiene that wherein chloroprene is 96.5% by weight fraction and weight fraction are 3.5%.
(2) polymerization: oil phase and water are placed in emulsifying kettle and after mixing and emulsifying, deliver to polymeric kettle at 20 ℃ by weight 1:1, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is 0.2:1; Then at 40 ℃, carry out polyreaction 2 hours, obtain latex;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is 0.15:1; Then latex is placed in chain rupture groove and carries out alkaline chain rupture, in latex relative density, reach at 1.068 o'clock and add terminator solution;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product; Wherein flocculation agent is comprised of the sodium-chlor of 0.55 weight part and the calcium chloride of 0.65 weight part.
Embodiment 2
(1) preparation: the chloroprene drying of 120 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.8 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 4.5 weight parts completely, and preparation obtains oil phase; The dispersion agent of 150 weight part softening waters, 0.75 weight part sodium hydroxide, 0.95 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 1.0 weight parts, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution; The 1-chloro-1,3-butadiene that the chlorbutadiene that wherein chloroprene is 96.5% by weight fraction and weight fraction are 3.5%.
(2) polymerization: oil phase and water are placed in emulsifying kettle and after mixing and emulsifying, deliver to polymeric kettle at 25 ℃ by weight 1:2, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is 0.35:1; Then at 45 ℃, carry out polyreaction 2.5 hours, obtain latex; In latex relative density, reach at 1.068 o'clock and add terminator solution;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is 0.3:1; Then latex is placed in and in chain rupture groove, carries out alkaline chain rupture;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product.Wherein flocculation agent is comprised of the sodium-chlor of 0.55 weight part and the calcium chloride of 0.65 weight part.
Embodiment 3
A preparation method for described chloroprene rubber, comprises the following steps:
(1) preparation: the chloroprene drying of 115 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.75 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 4 weight parts completely, and preparation obtains oil phase; The dispersion agent of 145 weight part softening waters, 0.7 weight part sodium hydroxide, 0.9 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 0.25 weight part, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution; The 1-chloro-1,3-butadiene that the chlorbutadiene that wherein chloroprene is 96.5% by weight fraction and weight fraction are 3.5%.
(2) polymerization: oil phase and water are placed in emulsifying kettle and after mixing and emulsifying, deliver to polymeric kettle at 23 ℃ by weight 1:1.5, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is 0.3:1; Then at 42 ℃, carry out polyreaction 2.5 hours, obtain latex; In latex relative density, reach at 1.068 o'clock and add terminator solution;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is 0.25:1; Then latex is placed in and in chain rupture groove, carries out alkaline chain rupture;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product; Wherein flocculation agent is comprised of the sodium-chlor of 0.55 weight part and the calcium chloride of 0.65 weight part.

Claims (5)

1. a preparation method for chloroprene rubber, comprises the following steps:
(1) preparation: the chloroprene drying of 100~120 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.6~0.8 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 3.5~4.5 weight parts completely, and preparation obtains oil phase; The dispersion agent of 130~150 weight part softening waters, 0.65~0.75 weight part sodium hydroxide, 0.85~0.95 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 0.2~1.0 weight part, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution;
(2) polymerization: by oil phase and water by weight 1:(1~2) be placed in emulsifying kettle at 20~25 ℃ after mixing and emulsifying, deliver to polymeric kettle, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is (0.2~0.35): 1; Then at 40~45 ℃, carry out polyreaction 2~2.5 hours, obtain latex;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is (0.15~0.3): 1; Then latex is placed in and in chain rupture groove, carries out alkaline chain rupture;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product.
2. the preparation method of chloroprene rubber according to claim 1, comprises the following steps:
(1) preparation: the chloroprene drying of 115 weight parts, cooling rear metering are sent into oil phase preparation still, the tert-dodecyl mercaptan of 0.75 weight part is added to oil phase preparation still, turn on agitator is stirred to dissolves the mersolates that adds again 4 weight parts completely, and preparation obtains oil phase; The dispersion agent of 145 weight part softening waters, 0.7 weight part sodium hydroxide, 0.9 weight part is uniformly mixed and is mixed with water; Preparation obtains the initiator solution of 0.25 weight part, the anthraquinone-2-sodium solution composition that the potassium persulfate solution that this initiator solution is 85% by weight fraction and weight fraction are 15%; 1.5 weight part ethylbenzene, 0.09 weight part antioxidant D TPD, 0.03 weight part sodium lauryl sulphate, 0.04 weight part beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt and 0.9 parts by weight of deionized water are uniformly mixed to preparation and obtain terminator solution;
(2) polymerization: oil phase and water are placed in emulsifying kettle and after mixing and emulsifying, deliver to polymeric kettle at 23 ℃ by weight 1:1.5, add the prepared initiator solution of step (1), wherein the weight ratio of initiator solution and oil phase is 0.3:1; Then at 42 ℃, carry out polyreaction 2.5 hours, obtain latex;
(3) termination and chain rupture: in the latex of step (2), add terminator solution to stop polyreaction, wherein the weight ratio of terminator solution and oil phase is 0.25:1; Then latex is placed in and in chain rupture groove, carries out alkaline chain rupture;
(4) cohesion and dry: the latex after alkaline chain rupture is placed in collection surface is condensed under flocculation agent effect, then through washing, extrusion dehydration, be dried, apply powder, cut to cut and obtain chloroprene rubber finished product.
3. according to the preparation method of chloroprene rubber described in claim 1 or 2, it is characterized in that the 1-chloro-1,3-butadiene that the chlorbutadiene that the chloroprene in described step (1) is 96.5% by weight fraction and weight fraction are 3.5%.
4. according to the preparation method of chloroprene rubber described in claim 1 or 2, it is characterized in that, in described step (3), in latex relative density, reach at 1.068 o'clock and add terminator solution.
5. according to the preparation method of chloroprene rubber described in claim 1 or 2, it is characterized in that, in described step (4), flocculation agent is comprised of the sodium-chlor of 0.55 weight part and the calcium chloride of 0.65 weight part.
CN201310546658.8A 2013-11-07 2013-11-07 Preparation method of chloroprene rubber Pending CN103570875A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864963A (en) * 2014-03-25 2014-06-18 北京化工大学 Preparation method for low-heat productivity natural rubber
CN107840985A (en) * 2017-10-25 2018-03-27 宝鸡圭彬光电设备有限公司 A kind of preparation method of power equipment electro-insulating rubber
CN109099825A (en) * 2018-09-29 2018-12-28 南通志乐新材料有限公司 A kind of new energy car battery recycling detection reuse means
CN111844767A (en) * 2018-11-20 2020-10-30 南通理工学院 Ultrasonic plastic welding machine and antifouling layer thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101284895A (en) * 2008-06-03 2008-10-15 重庆长寿化工有限责任公司 Neoprene, method for preparing same and applications

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101284895A (en) * 2008-06-03 2008-10-15 重庆长寿化工有限责任公司 Neoprene, method for preparing same and applications

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864963A (en) * 2014-03-25 2014-06-18 北京化工大学 Preparation method for low-heat productivity natural rubber
CN103864963B (en) * 2014-03-25 2015-12-09 北京化工大学 A kind of preparation method of low-heat-generation natural rubber
CN107840985A (en) * 2017-10-25 2018-03-27 宝鸡圭彬光电设备有限公司 A kind of preparation method of power equipment electro-insulating rubber
CN109099825A (en) * 2018-09-29 2018-12-28 南通志乐新材料有限公司 A kind of new energy car battery recycling detection reuse means
CN111844767A (en) * 2018-11-20 2020-10-30 南通理工学院 Ultrasonic plastic welding machine and antifouling layer thereof

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Application publication date: 20140212