CN101225068B - Method for preparing vulcanizing agent 3,4-dichlorobenzoyl peroxide - Google Patents
Method for preparing vulcanizing agent 3,4-dichlorobenzoyl peroxide Download PDFInfo
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- CN101225068B CN101225068B CN2008100205398A CN200810020539A CN101225068B CN 101225068 B CN101225068 B CN 101225068B CN 2008100205398 A CN2008100205398 A CN 2008100205398A CN 200810020539 A CN200810020539 A CN 200810020539A CN 101225068 B CN101225068 B CN 101225068B
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- dichlorobenzoperoxide
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- dichlorobenzoyl chloride
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Abstract
The invention relates to a preparation method for the vulcanizing agent of 3, 4-dichloro benzoyl peroxide, belonging to the technical field of vulcanizing agent preparation, which comprises the steps as follows: A) sodium hydroxide solution, hydrogen peroxide, water, surfactant and solvent are put in a reaction device and stirred, and the temperature is adjusted to obtain the base material for reaction; B) 3, 4-dichloro benzoyl chloride is added into the base material for reaction, and thermal insulation is conducted to obtain the reactant; C) the reactant is separated, then washed, dried again to obtain the 3, 4-dichloro benzoyl peroxide, finally the 3, 4-dichloro benzoyl peroxide is kneaded and ground to obtain the finished product of paste-shaped vulcanizing agent of 3, 4-dichloro benzoyl peroxide; wherein, the diluent is added in at least in one or more than one of the A), B) and C) steps. The preparation method for the vulcanizing agent of 3, 4-dichloro benzoyl peroxide has the advantages that process steps are simple; equipment using and process requirements are not strict; and the obtained finished product has good stability which provides safety guarantee for storage, transportation and application and which is beneficial to utilization and popularization of the product.
Description
Technical field
The invention belongs to the preparing technical field of vulcanizing agent, be specifically related to a kind of vulcanizing agent 3, the preparation method of 4-dichlorobenzoperoxide.
Background technology
3, the English name of 4-dichlorobenzoperoxide is: 3, and 4-dichloro benzoyl peroxide.Its molecular formula is: C
14H
6Cl
4O
4Molecular weight is: 380.10; Structural formula is:
3, it is two three or four that the 4-dichlorobenzoperoxide abbreviates as, is diacyl organic peroxide, is a kind of free radical donor, and as auxiliary chemicals, the mechanism of action is: its peroxy-radical-O-O-can be decomposed to form two free radicals by the homolysis of bonding sharing electron.Before, existing 3, (the applicant proposes, and application number is: 200810019045.8), its preparation method is introduced in the preparation method's of 4-dichlorobenzoperoxide patent application.But, two 34 is a kind of unsettled materials, owing to be heated even under quite low temperature, also can decomposing, thereby bring potential safety hazard for transportation, storage and processing, therefore, generally not with 3, the 4-dichlorobenzoperoxide is directly as sale of finished goods, unless take harsh transportation, storage and processing measure.For the ease of making 3, therefore the 4-dichlorobenzoperoxide must dilute it as commodity selling, its concentration is reduced to have the high degree of self-accelerating decomposition temperature and uses and reach transportation, storage purpose of safety.The technical scheme that the present invention will introduce below is based on producing under this background.
Summary of the invention
Task of the present invention be to provide a kind of self-accelerating decomposition temperature high and use ensure transportation, store safety, technology is simple, the vulcanizing agent 3 being convenient to use, the preparation method of 4-dichlorobenzoperoxide.
Task of the present invention is finished like this, a kind of vulcanizing agent 3, and the preparation method of 4-dichlorobenzoperoxide, it may further comprise the steps:
A) sodium hydroxide solution, hydrogen peroxide, water, tensio-active agent, solvent are put in the reaction unit and stirred, and adjust temperature to 0～31 ℃, obtain reacting the base-material of usefulness;
B) with 3, the 4-dichlorobenzoyl chloride adds in the base-material of reaction usefulness, and insulation, obtains reactant;
C) to reactants separate, washing then, dry again, obtain 3, the 4-dichlorobenzoperoxide, at last to 3, the 4-dichlorobenzoperoxide is mediated, is ground, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, wherein: at above-mentioned A), B), C) add at least one or the more than one step in three steps thinner arranged, wherein: described solvent is a varsol, described varsol is any one in benzene, toluene, Benzene Chloride, hexane, hexanaphthene, heptane, octane, the ethylene dichloride; Described thinner is any one in silicone oil, white oil, the softening agent; Described softening agent is any one among DBP, DIBP, DOP, the DIOP.
In a specific embodiment of the present invention, described thinner and 3, the weight ratio of 4-dichlorobenzoyl chloride is 0.447～16.11: 1, wherein: when described thinner and 3, the weight ratio of 4-dichlorobenzoyl chloride is also to add that filler, described filler are arranged is silicon-dioxide at 4～16.11: 1 o'clock when mediating.
In another specific embodiment of the present invention, described 3, the weight ratio of 4-dichlorobenzoyl chloride and filler is 1: 0.08～0.18.
More of the present invention and in specific embodiment, described sodium hydroxide solution, hydrogen peroxide, 3, the mol ratio of 4-dichlorobenzoyl chloride is 1.48～2.0: 0.98～1.48: 1; Described water, tensio-active agent, solvent, 3, the weight ratio of 4-dichlorobenzoyl chloride are 2.5～4.2: 0.08～0.17: 0.8～2.5: 1; Described 3, the purity of 4-dichlorobenzoyl chloride is technical grade purity.
In of the present invention and then specific embodiment, described 3, the adding mode that the 4-dichlorobenzoyl chloride joins in the base-material of reaction usefulness is dropping, and the dropping time is 〉=15min; The holding temperature of described insulation is 0～35 ℃, and soaking time is 〉=15min; Described exsiccant drying temperature is≤40 ℃.
Of the present invention again more and in specific embodiment, described tensio-active agent is any one among Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium laurylsulfonate, the PEG-2000.
Brief by the inventive method processing step, use equipment and processing requirement are not harsh, and resulting finished product stability is good, provide safety control for storing, transport, using, and help the utilization and the popularization of this product.
Embodiment
Embodiment 1
A) drop into sodium hydroxide solution 8.362mol, hydrogen peroxide 5.537mol, water 3000g, sodium laurylsulfonate 96g, toluene 960g, silicone oil 497g in the reactor, stir, adjust temperature to 0 ℃, obtain reacting the base-material of usefulness;
B) be 3 of technical grade with purity, 4-dichlorobenzoyl chloride 5.65mol (1200g) is added drop-wise in the base-material of reaction usefulness in the dropping mode, and dropping temperature maintains 0～5 ℃, drips time 15min, drips the end back and keeps reaction 200min at 35 ℃, obtains reactant;
C) in filtering mode with reactants separate, washing obtains 3,4-dichlorobenzoperoxide tide product (product wet), with the tide product in moisture eliminator in 35 ℃ of dry 5h, obtain 3, the 4-dichlorobenzoperoxide is fully mediated in kneader, is ground evenly, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, after testing, 3,4-dichlorobenzoperoxide content 79.6%, active o content 3.36%.
Embodiment 2
A) in reactor, drop into sodium hydroxide solution 9.605mol, hydrogen peroxide 7.062mol, water 3600g, sodium laurylsulfonate 180g, hexane 1440g, stir, adjust temperature to 12 ℃, obtain reacting the base-material of usefulness;
B) be 3 of technical grade with purity, 4-dichlorobenzoyl chloride 5.65mol (1200g) is added drop-wise in the base-material of reaction usefulness in the dropping mode, and dropping temperature maintains 10～15 ℃, dropping time 55min, drip and finish back adding white oil 1285g, keep reaction 110min, obtain reactant at 15 ℃;
C) the reactant layering is separated, washing obtains 3,4-dichlorobenzoperoxide tide product, with the tide product in moisture eliminator in 40 ℃ of dry 5h, obtain 3, the 4-dichlorobenzoperoxide, and it is put in the kneader fully mediate, grind evenly, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, after testing, 3,4-dichlorobenzoperoxide content 60.42%, active o content 2.55%.
Embodiment 3
A) in reactor, drop into sodium hydroxide solution 10.735mol, hydrogen peroxide 6.215mol, water 5040g, SDS 204g, ethylene dichloride 3000g, silicone oil 1000g, stir, adjust temperature to 20 ℃, obtain reacting the base-material of usefulness;
B) be 3 of technical grade purity with purity, 4-dichlorobenzoyl chloride 5.65mol (1200g) is added drop-wise in the base-material of reaction usefulness in the dropping mode, and dropping temperature maintains 20～24 ℃, dropping time 92min, add silicone oil 1011g again after dripping end, keep reaction 42min, obtain reactant at 28 ℃;
C) the reactant layering is separated, washing obtains 3,4-dichlorobenzoperoxide tide product, with the tide product in moisture eliminator in dry 5h below 38 ℃, obtain 3, the 4-dichlorobenzoperoxide changes in the kneader and fully mediates, grinds evenly, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, after testing, 3,4-dichlorobenzoperoxide content 49.56%, active o content 2.09%.
Embodiment 4
A) in reactor, drop into sodium hydroxide solution 11.30mol, hydrogen peroxide 8.362mol, water 4800g, PEG-2000 (polyoxyethylene glycol-2000) 125g, hexanaphthene 2300g, DBP1800g, stir, adjust temperature to 31 ℃, obtain reacting the base-material of usefulness;
B) be 3 of technical grade with purity, 4-dichlorobenzoyl chloride 5.65mol (1200g) is added drop-wise in the base-material of reaction usefulness in the dropping mode, and dropping temperature maintains 31～35 ℃, drips time 135min, drip and finish the back, obtain reactant at 33 ℃ of maintenance reaction 15min;
C) the reactant layering is separated, washing obtains 3,4-dichlorobenzoperoxide tide product, with the tide product in moisture eliminator in 40 ℃ of dry 5h, obtain 3, the 4-dichlorobenzoperoxide, and it is changed in the kneader, add DBP3000g, silicon-dioxide 96g, fully mediate, grind evenly, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, after testing, 3,4-dichlorobenzoperoxide content 28.65%, active o content 1.21%.
Embodiment 5
A) in reactor, drop into sodium hydroxide solution 10.735mol, hydrogen peroxide 6.215mol, water 5040g, sodium laurylsulfonate 204g, hexanaphthene 3000g, DOP 2500g, stir, adjust temperature to 20 ℃, obtain reacting the base-material of usefulness;
B) be 3 of technical grade purity with purity, 4-dichlorobenzoyl chloride 5.65mol (1200g) is added drop-wise in the base-material of reaction usefulness in the dropping mode, and dropping temperature maintains 20～24 ℃, dropping time 92min, add DOP 2500g again after dripping end, keep reaction 42min, obtain reactant at 28 ℃;
C) with the reactant layering, washing obtains 3,4-dichlorobenzoperoxide tide product, with the tide product in moisture eliminator in dry 6h below 38 ℃, obtain 3, the 4-dichlorobenzoperoxide changes in the kneader again and to add DOP 5500g, silica 1 45g and fully mediate, grind evenly, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, after testing, 3,4-dichlorobenzoperoxide content 15.42%, active o content 0.65%.
Embodiment 6
A) in reactor, drop into sodium hydroxide solution 10.735mol, hydrogen peroxide 6.215mol, water 5040g, Sodium dodecylbenzene sulfonate 200g, benzene 3000g, DIBP 2000g, stir, adjust temperature to 20 ℃, obtain reacting the base-material of usefulness;
B) be 3 of technical grade with purity, 4-dichlorobenzoyl chloride 5.65mol (1200g) is added drop-wise in the base-material of reaction usefulness in the dropping mode, and dropping temperature maintains 20～24 ℃, drips time 92min, drips to finish to keep reaction 42min at 28 ℃, obtains reactant;
C) with the reactant layering, washing obtains 3,4-dichlorobenzoperoxide tide product, with the tide product in moisture eliminator in dry 6h below 38 ℃, obtain 3, the 4-dichlorobenzoperoxide changes in the kneader again and to add DIBP 17332g, silicon-dioxide 216g and fully mediate, grind evenly, obtain the vulcanizing agent 3 of paste, 4-dichlorobenzoperoxide finished product, after testing, 3,4-dichlorobenzoperoxide content 9.11%, active o content 0.39%.
Claims (6)
1. vulcanizing agent 3, the preparation method of 4-dichlorobenzoperoxide is characterized in that it may further comprise the steps:
A) base-material of preparation reaction usefulness is put into sodium hydroxide solution, hydrogen peroxide, water, tensio-active agent, solvent in the reaction unit and is stirred, and adjusts temperature to 0～31 ℃, obtains reacting the base-material of usefulness;
B) material reaction, with 3, the 4-dichlorobenzoyl chloride adds in the base-material of reaction usefulness, and insulation, obtains reactant;
C) to the reactant aftertreatment, earlier to reactants separate, washing then, drying, kneading, grinding again, obtain finished product vulcanizing agent 3, the 4-dichlorobenzoperoxide, wherein: at above-mentioned A), B), C) add at least one or the more than one step in three steps thinner arranged, wherein: described solvent is a varsol, and described varsol is any one in benzene, toluene, Benzene Chloride, hexane, hexanaphthene, heptane, octane, the ethylene dichloride; Described thinner is any one in silicone oil, white oil, the softening agent; Described softening agent is any one among DBP, DIBP, DOP, the DIOP.
2. a kind of vulcanizing agent 3 according to claim 1, the preparation method of 4-dichlorobenzoperoxide, it is characterized in that described thinner and 3 of reaction usefulness, the weight ratio of 4-dichlorobenzoyl chloride is 0.447～16.11: 1, wherein: when described thinner and 3 of reaction usefulness, the weight ratio of 4-dichlorobenzoyl chloride is also to add that filler, described filler are arranged is silicon-dioxide at 4～16.11: 1 o'clock when mediating.
3. a kind of vulcanizing agent 3 according to claim 2, the preparation method of 4-dichlorobenzoperoxide is characterized in that describedly 3, the weight ratio of 4-dichlorobenzoyl chloride and filler is 1: 0.08～0.18.
4. a kind of vulcanizing agent 3 according to claim 1, the preparation method of 4-dichlorobenzoperoxide is characterized in that described sodium hydroxide solution, hydrogen peroxide, 3, the mol ratio of 4-dichlorobenzoyl chloride is 1.48～2.0: 0.98～1.48: 1; Described water, tensio-active agent, solvent, 3, the weight ratio of 4-dichlorobenzoyl chloride are 2.5～4.2: 0.08～0.17: 0.8～2.5: 1; Described 3, the purity of 4-dichlorobenzoyl chloride is technical grade purity.
5. a kind of vulcanizing agent 3 according to claim 1, the preparation method of 4-dichlorobenzoperoxide is characterized in that describedly 3, and the adding mode that the 4-dichlorobenzoyl chloride joins in the base-material of reaction usefulness is dropping, and the dropping time is 〉=15min; The holding temperature of described insulation is 0～35 ℃, and soaking time is 〉=15min; Described exsiccant drying temperature is≤40 ℃.
6. a kind of vulcanizing agent 3 according to claim 1, the preparation method of 4-dichlorobenzoperoxide is characterized in that described tensio-active agent is any one among Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium laurylsulfonate, the PEG-2000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100205398A CN101225068B (en) | 2008-01-29 | 2008-01-29 | Method for preparing vulcanizing agent 3,4-dichlorobenzoyl peroxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100205398A CN101225068B (en) | 2008-01-29 | 2008-01-29 | Method for preparing vulcanizing agent 3,4-dichlorobenzoyl peroxide |
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| Publication Number | Publication Date |
|---|---|
| CN101225068A CN101225068A (en) | 2008-07-23 |
| CN101225068B true CN101225068B (en) | 2010-08-11 |
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| CN2008100205398A Active CN101225068B (en) | 2008-01-29 | 2008-01-29 | Method for preparing vulcanizing agent 3,4-dichlorobenzoyl peroxide |
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Owner name: CHINASUN SPECIALTY PRODUCTS CO., LTD Free format text: FORMER NAME: JIANGSU QIANGSHENG CHEMICAL CO., LTD. |
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Address after: 215532 Jiangsu province Changshou City Baimao Industrial Economic Development Zone Patentee after: Jiangsu Chinasun Specialty Products Co.,Ltd. Address before: The ancient town of Changshou City province Jiangsu 215532 Baimao Industrial Economic Development Zone Patentee before: Jiangsu Qiangsheng Chemical Co., Ltd. |