CN103113206A - Preparation method of neodecanoic acid cobalt - Google Patents

Preparation method of neodecanoic acid cobalt Download PDF

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Publication number
CN103113206A
CN103113206A CN2012105909191A CN201210590919A CN103113206A CN 103113206 A CN103113206 A CN 103113206A CN 2012105909191 A CN2012105909191 A CN 2012105909191A CN 201210590919 A CN201210590919 A CN 201210590919A CN 103113206 A CN103113206 A CN 103113206A
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acid
dimethylbenzene
preparation
new cobalt
reaction
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马侠
孙延亮
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Dalian Advance Performance Specialty Chemicals Co Ltd
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Dalian Advance Performance Specialty Chemicals Co Ltd
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Priority to CN2012105909191A priority Critical patent/CN103113206A/en
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Abstract

The invention discloses a preparation method of neodecanoic acid cobalt. The method comprises the following steps that: neodecanoic acid, propionic acid, stearic acid, valeric acid, dimethylbenzene and cobaltous hydroxide are mixed to carry out an acid-base neutralization reaction; and after the reaction is finished, the neodecanoic acid cobalt as a product is obtained. The method is simple to operate. The indexes of the prepared neodecanoic acid cobalt all conform to the production requirements of manufacturers.

Description

A kind of preparation method of new cobalt decanoate
Technical field
The present invention relates to the preparing technical field of Chemicals, relate in particular to a kind of preparation method who can be used as the new cobalt decanoate of rubber adhesion accelerating agent.
Background technology
Current, cobalt salt class tackiness agent still is divided into diacid cobalt and the large series products of cobalt boracylate two both at home and abroad.Cobalt boracylate is as novel cobalt salt adhesion promotion agent, and its excellent properties is recognized the world over.But due to the restriction that filled a prescription separately by tyre industry; diacid cobalt salt class adhesionpromoter can not all be replaced by cobalt boracylate in radial tyre is produced; particularly as the development success of diacid cobalt salt series products of new generation-capric acid cobalt, its excellent performance more is subject to the favor of world's rubber circle.
Typical diacid cobalt salt, in molecular composition, acid/cobalt molecular ratio is 2: 1, and the acid of capric acid cobalt/cobalt mole ratio is 1.69: 1, this shows the common single cobalt class-C of existing diacid cobalt-O-Co-O-C-associative key in the molecular composition of capric acid cobalt, also existence-C-O-Co-O-Co-O-C-two cobalt class associative keys.Under cure conditions, this pair of weak associative key of cobalt class more easily emitted active cobalt and generates rapidly cobaltous sulfide than the bonding of single cobalt class, and this special molecular linkage is that the capric acid cobalt is than the high major cause of common diacid cobalt reactive behavior.
Studies show that, be neodecanoic acid with two side chains in order to the acid of synthetic capric acid cobalt salt, because branched chain length carbochain acid cobalt salt has better intermiscibility than the long carbochain acid of straight chain cobalt salt in rubber, thereby its processing performance when mixing is more much better than the common diacid cobalt of use.
The key technical indexes of mentioning in the national standard of new cobalt decanoate is cobalt contents, weight loss on heating and softening temperature, its softening temperature is the most important index of new cobalt decanoate, relation next step use in mixing process, the new cobalt decanoate that softening temperature is low is easier to be disperseed in rubber, reaches desirable refining glue effect.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of new cobalt decanoate, the new cobalt decanoate softening temperature that makes is low, meets the production requirement of tire producer.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of new cobalt decanoate comprises:
Neodecanoic acid, propionic acid, stearic acid, valeric acid, dimethylbenzene are mixed with cobaltous hydroxide carry out the acid-base neutralisation reaction, the product that obtains after reaction is completed is new cobalt decanoate.
The content weight ratio of described neodecanoic acid, propionic acid, stearic acid, valeric acid, dimethylbenzene and cobaltous hydroxide is:
Neodecanoic acid: 50~55 parts;
Propionic acid: 19~21 parts;
Stearic acid: 4~8 parts;
Valeric acid: 40~50 parts;
Dimethylbenzene: 0~4 part;
Cobaltous hydroxide: 30~34 parts.
Described stearic acid is stearic acid 1845.
The acid number of described stearic acid 1845 is 205~210.
Described neutralization reaction comprises:
After neodecanoic acid, propionic acid, stearic acid 1845, valeric acid and dimethylbenzene are mixed, add cobaltous hydroxide under the state that stirring vacuumizes;
After cobaltous hydroxide added, when being warming up to 85~95 ℃, dimethylbenzene and water were discharged in distillation;
When being warming up to 155~165 ℃, carry out underpressure distillation, in vacuum distillation process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps 120 minutes under vacuum tightness-0.08MPa, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.
Described neodecanoic acid, propionic acid, stearic acid 1845, valeric acid and dimethylbenzene are mixed after, add cobaltous hydroxide under the state that stirring vacuumizes, specifically comprise:
Neodecanoic acid, propionic acid, stearic acid, valeric acid and dimethylbenzene are joined in reactor, start high-speed stirring, 150~250 rev/mins of stirring velocitys stir and to add at a slow speed cobaltous hydroxide to carry out the acid-base neutralisation reaction simultaneously, add temperature reaction after cobaltous hydroxide; When temperature rose to 93 ℃, dimethylbenzene and water were discharged in distillation.
Describedly carry out underpressure distillation, in vacuum distillation process vacuum tightness from-0.01MPa be down to-0.08MPa comprises:
After entering underpressure distillation, vacuum tightness is from-0.01MPa, and every 10 minutes reduction-0.01MPa are until vacuum tightness is down to-0.08MPa.
The preparation method of described new cobalt decanoate also comprises:
The step that the reaction product that obtains after reaction is completed to acid-base neutralisation is carried out granulation adopts the rotary-belt condensation granulator, and the cooling temperature of granulation is 25~35 ℃.
As seen from the above technical solution provided by the invention, the preparation method of a kind of new cobalt decanoate that the embodiment of the present invention provides, simple to operate, the new cobalt decanoate index that makes all meets the production requirement of producer.
Embodiment
The below is clearly and completely described the technical scheme in the embodiment of the present invention, and obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills belong to protection scope of the present invention not making the every other embodiment that obtains under the creative work prerequisite.
The below is described in further detail the embodiment of the present invention.
Embodiment one
The present embodiment provides a kind of preparation method of new cobalt decanoate, can be used as well behaved rubber composite promotor, and the method comprises:
Neodecanoic acid, propionic acid, stearic acid 1845, valeric acid, dimethylbenzene are mixed with cobaltous hydroxide carry out the acid-base neutralisation reaction, the product that obtains after neutralization reaction is completed is new cobalt decanoate;
Concrete steps: after neodecanoic acid, propionic acid, stearic acid 1845, valeric acid, dimethylbenzene are mixed, add cobaltous hydroxide under the state that stirring vacuumizes; After cobaltous hydroxide added, when being warming up to 85~95 ℃, dimethylbenzene and water were discharged in distillation; When being warming up to 155~165 ℃, carry out underpressure distillation, in decompression process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps under vacuum tightness-0.08MPa after 120 minutes, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.
For make the new cobalt decanoate that makes instant packed with use, can further carry out granulation to the reaction product that obtains after reaction, as, can adopt the rotary-belt condensation granulator to carry out granulation, the cooling temperature of granulation is 25~35 ℃.Making granular new cobalt decanoate is easier to packing and adds in producing rubber composite.[0017] in aforesaid method, the content weight ratio of controlling each raw material by following weight proportion is:
Neodecanoic acid: 50~55 parts;
Propionic acid: 19~21 parts;
Stearic acid: 4~8 parts;
Valeric acid: 40~50 parts;
Dimethylbenzene: 0~4 part;
Cobaltous hydroxide: 30~34 parts.
In the preparation method of the embodiment of the present invention, neodecanoic acid, 1,845 two kinds of higher fatty acid of stearic acid and lower fatty acid propionic acid, valeric acid are together, with cobaltous hydroxide generation acid-base neutralisation reaction, improve speed of reaction, stearic acid 1845 and valeric acid add the new cobalt decanoate softening temperature that makes generation low.
Embodiment two
The present embodiment provides a kind of preparation method of new cobalt decanoate, and the new cobalt decanoate that makes can be used as rubber combined promotor, and the method comprises:
The dimethylbenzene of the propionic acid of the neodecanoic acid of 50~55 weight parts, 19~21 weight parts, 4 weight part stearic acid 1845,1~3 weight part valeric acid, 40~50 weight parts is joined in reactor, start the cobaltous hydroxide that high-speed stirring (150~250 rev/mins) adds at a slow speed simultaneously 30~34 weight parts and carry out the acid-base neutralisation reaction, add temperature reaction after cobaltous hydroxide; When temperature rose to 93 ℃, dimethylbenzene and water were discharged in distillation;
When being warming up to 160 ℃, carry out underpressure distillation, in decompression process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps under vacuum tightness-0.08MPa after 120 minutes, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.This new cobalt decanoate can be used as rubber composite promotor, and its performance test results is seen Table 1.
It is more convenient when the new cobalt decanoate that makes is used as rubber composite promotor; the product that can further make above-mentioned neutralization reaction carries out granulation to be processed; as carrying out granulation by the rotary-belt condensation granulator; the cooling temperature of granulation is 30 ℃ of left and right; granulation can obtain the new cobalt decanoate particle after processing.Granular new cobalt decanoate adds when being easy to packing and rubber composite production.
Embodiment three
The present embodiment provides a kind of preparation method of new cobalt decanoate, and the new cobalt decanoate that makes can be used as rubber combined promotor, and the method comprises:
The dimethylbenzene of the propionic acid of the neodecanoic acid of 50~55 weight parts, 19~21 weight parts, 8 weight part stearic acid 1845,1~3 weight part valeric acid, 40~50 weight parts is joined in reactor, start the cobaltous hydroxide that high-speed stirring (150~250 rev/mins) adds at a slow speed simultaneously 30~34 weight parts and carry out the acid-base neutralisation reaction, add temperature reaction after cobaltous hydroxide; When temperature rose to 93 ℃, dimethylbenzene and water were discharged in distillation;
When being warming up to 160 ℃, carry out underpressure distillation, in decompression process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps under vacuum tightness-0.08MPa after 120 minutes, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.This new cobalt decanoate can be used as rubber composite promotor, and its performance test results is seen Table 1.
It is more convenient when the new cobalt decanoate that makes is used as rubber composite promotor; the product that can further make above-mentioned neutralization reaction carries out granulation to be processed; as carrying out granulation by the rotary-belt condensation granulator; the cooling temperature of granulation is 30 ℃ of left and right; granulation can obtain the new cobalt decanoate particle after processing.Granular new cobalt decanoate adds when being easy to packing and rubber composite production.
Embodiment four
The present embodiment provides a kind of preparation method of new cobalt decanoate, and the new cobalt decanoate that makes can be used as rubber combined promotor, and the method comprises:
The dimethylbenzene of the propionic acid of the neodecanoic acid of 50~55 weight parts, 19~21 weight parts, 5~7 weight part stearic acid 1845,0 weight part valeric acid, 40~50 weight parts is joined in reactor, start the cobaltous hydroxide that high-speed stirring (150~250 rev/mins) adds at a slow speed simultaneously 30~34 weight parts and carry out the acid-base neutralisation reaction, add temperature reaction after cobaltous hydroxide; When temperature rose to 93 ℃, dimethylbenzene and water were discharged in distillation;
When being warming up to 160 ℃, carry out underpressure distillation, in decompression process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps under vacuum tightness-0.08MPa after 120 minutes, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.This new cobalt decanoate can be used as rubber composite promotor, and its performance test results is seen Table 1.
It is more convenient when the new cobalt decanoate that makes is used as rubber composite promotor; the product that can further make above-mentioned neutralization reaction carries out granulation to be processed; as carrying out granulation by the rotary-belt condensation granulator; the cooling temperature of granulation is 30 ℃ of left and right; granulation can obtain the new cobalt decanoate particle after processing.Granular new cobalt decanoate adds when being easy to packing and rubber composite production.
Embodiment five
The present embodiment provides a kind of preparation method of new cobalt decanoate, and the new cobalt decanoate that makes can be used as rubber combined promotor, and the method comprises:
The dimethylbenzene of the propionic acid of the neodecanoic acid of 50~55 weight parts, 19~21 weight parts, 5~7 weight part stearic acid 1845,4 weight part valeric acids, 40~50 weight parts is joined in reactor, start the cobaltous hydroxide that high-speed stirring (150~250 rev/mins) adds at a slow speed simultaneously 30~34 weight parts and carry out the acid-base neutralisation reaction, add temperature reaction after cobaltous hydroxide; When temperature rose to 93 ℃, dimethylbenzene and water were discharged in distillation;
When being warming up to 160 ℃, carry out underpressure distillation, in decompression process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps under vacuum tightness-0.08MPa after 120 minutes, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.This new cobalt decanoate can be used as rubber composite promotor, and its performance test results is seen Table 1.
It is more convenient when the new cobalt decanoate that makes is used as rubber composite promotor; the product that can further make above-mentioned neutralization reaction carries out granulation to be processed; as carrying out granulation by the rotary-belt condensation granulator; the cooling temperature of granulation is 30 ℃ of left and right; granulation can obtain the new cobalt decanoate particle after processing.Granular new cobalt decanoate adds when being easy to packing and rubber composite production.
Each embodiment of table 1 makes new cobalt decanoate performance test table
Sequence number Cobalt contents (%) Weight loss on heating (%) Softening temperature (℃)
Embodiment one 20.52 0.30 94
Embodiment two 20.60 0.28 102
Embodiment three 20.45 0.35 100
Embodiment four 20.55 0.30 104
Embodiment five 20.45 0.36 98
The new cobalt decanoate for preparing in the embodiment of the present invention can be used as rubber composite promotor, shows high reactivity under vulcanization of rubber condition, and softening temperature is low, is conducive to the Uniform Dispersion of cobalt salt in mixing process.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement are within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.

Claims (8)

1. the preparation method of a new cobalt decanoate, is characterized in that, comprising:
Neodecanoic acid, propionic acid, stearic acid, valeric acid, dimethylbenzene are mixed with cobaltous hydroxide carry out the acid-base neutralisation reaction, the product that obtains after reaction is completed is new cobalt decanoate.
2. according to the preparation method of new cobalt decanoate claimed in claim 1, it is characterized in that, the content weight ratio of described neodecanoic acid, propionic acid, stearic acid, valeric acid, dimethylbenzene and cobaltous hydroxide is:
Neodecanoic acid: 50~55 parts;
Propionic acid: 19~21 parts;
Stearic acid: 4~8 parts;
Valeric acid: 40~50 parts;
Dimethylbenzene: 0~4 part;
Cobaltous hydroxide: 30~34 parts.
3. according to the preparation method of new cobalt decanoate claimed in claim 2, it is characterized in that, described stearic acid is stearic acid 1845.
4. according to the preparation method of new cobalt decanoate claimed in claim 3, it is characterized in that, the acid number of described stearic acid 1845 is 205~210.
5. according to the preparation method of claim 1,2,3 or 4 described new cobalt decanoates, it is characterized in that, described neutralization reaction comprises:
After neodecanoic acid, propionic acid, stearic acid 1845, valeric acid and dimethylbenzene are mixed, add cobaltous hydroxide under the state that stirring vacuumizes;
After cobaltous hydroxide added, when being warming up to 85~95 ℃, dimethylbenzene and water were discharged in distillation;
When being warming up to 155~165 ℃, carry out underpressure distillation, in vacuum distillation process, vacuum tightness is down to-0.08MPa from-0.01MPa, and keeps 120 minutes under vacuum tightness-0.08MPa, completes the product that the acid-base neutralisation reaction obtains and is new cobalt decanoate.
6. according to the preparation method of new cobalt decanoate claimed in claim 5, it is characterized in that, described neodecanoic acid, propionic acid, stearic acid 1845, valeric acid and dimethylbenzene are mixed after, add cobaltous hydroxide under the state that stirring vacuumizes, specifically comprise:
Neodecanoic acid, propionic acid, stearic acid, valeric acid and dimethylbenzene are joined in reactor, start high-speed stirring, 150~250 rev/mins of stirring velocitys stir and to add at a slow speed cobaltous hydroxide to carry out the acid-base neutralisation reaction simultaneously, add temperature reaction after cobaltous hydroxide; When temperature rose to 93 ℃, dimethylbenzene and water were discharged in distillation.
7. according to the preparation method of new cobalt decanoate claimed in claim 5, it is characterized in that, describedly carry out underpressure distillation, in vacuum distillation process vacuum tightness from-0.01M Pa be down to-0.08M Pa comprises:
After entering underpressure distillation, vacuum tightness is from-0.01MPa, and every 10 minutes reduction-0.01MPa are until vacuum tightness is down to-0.08MPa.
8. according to the preparation method of new cobalt decanoate claimed in claim 1, it is characterized in that, described method also comprises:
The step that the reaction product that obtains after reaction is completed to acid-base neutralisation is carried out granulation adopts the rotary-belt condensation granulator, and the cooling temperature of granulation is 25~35 ℃.
CN2012105909191A 2012-12-31 2012-12-31 Preparation method of neodecanoic acid cobalt Pending CN103113206A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104788718A (en) * 2015-04-15 2015-07-22 江阴市三良化工有限公司 Preparation method for high-stability cobalt neocaprate mixed salt
CN107011369A (en) * 2017-04-18 2017-08-04 江阴市三良橡塑新材料有限公司 A kind of preparation method of high-performance compound cobalt boracylate
CN110092942A (en) * 2019-05-08 2019-08-06 国运科技(大连)有限公司 A kind of novel cobaltous octadecanate adhesion promotor and preparation method improving cobalt content

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US5276172A (en) * 1990-07-10 1994-01-04 Rhone-Poulenc Chemicals Ltd. Metal organic compounds
CN101333160A (en) * 2008-07-18 2008-12-31 镇江迈特化工新材料有限责任公司 Process for synthesizing new cobalt decanoate
CN101481591A (en) * 2009-02-09 2009-07-15 宜兴市卡欧化工有限公司 Preparation of organic cobalt salt adhesion promotion agent
CN101805253A (en) * 2010-04-01 2010-08-18 镇江迈特化工新材料有限责任公司 Method for synthesizing cobalt neocaprate through water solvent
CN101864088A (en) * 2010-06-13 2010-10-20 宜兴市卡欧化工有限公司 Preparation method of compound type cobalt stearate adhesion promoter
CN102432452A (en) * 2011-09-30 2012-05-02 西南化工研究设计院 Method for preparing C10 cobalt neodecanoate rubber adhesive promoter

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5276172A (en) * 1990-07-10 1994-01-04 Rhone-Poulenc Chemicals Ltd. Metal organic compounds
CN101333160A (en) * 2008-07-18 2008-12-31 镇江迈特化工新材料有限责任公司 Process for synthesizing new cobalt decanoate
CN101481591A (en) * 2009-02-09 2009-07-15 宜兴市卡欧化工有限公司 Preparation of organic cobalt salt adhesion promotion agent
CN101805253A (en) * 2010-04-01 2010-08-18 镇江迈特化工新材料有限责任公司 Method for synthesizing cobalt neocaprate through water solvent
CN101864088A (en) * 2010-06-13 2010-10-20 宜兴市卡欧化工有限公司 Preparation method of compound type cobalt stearate adhesion promoter
CN102432452A (en) * 2011-09-30 2012-05-02 西南化工研究设计院 Method for preparing C10 cobalt neodecanoate rubber adhesive promoter

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104788718A (en) * 2015-04-15 2015-07-22 江阴市三良化工有限公司 Preparation method for high-stability cobalt neocaprate mixed salt
CN104788718B (en) * 2015-04-15 2017-07-18 江阴市三良橡塑新材料有限公司 A kind of high stability new cobalt decanoate mixing salt production process
CN107011369A (en) * 2017-04-18 2017-08-04 江阴市三良橡塑新材料有限公司 A kind of preparation method of high-performance compound cobalt boracylate
CN110092942A (en) * 2019-05-08 2019-08-06 国运科技(大连)有限公司 A kind of novel cobaltous octadecanate adhesion promotor and preparation method improving cobalt content

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