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A kind of clean production method of tetrabenzylthiuram disulfide

A technology of tetrabenzylthiuram disulfide and production method, applied in directions such as organic chemistry, can solve problems such as recycling, increase production cost of waste water treatment and environmental pollution, and achieve reduction in production cost and pale yellow appearance , The effect of reducing the hidden danger of process safety

Active Publication Date: 2021-01-22
SHANDONG YANGGU HUATAI CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mother liquor wastewater produced by this method cannot be recycled in the next batch, which increases the production cost and environmental pollution problems caused by wastewater treatment

Method used

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  • A kind of clean production method of tetrabenzylthiuram disulfide
  • A kind of clean production method of tetrabenzylthiuram disulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Weigh each raw material: 100g of dibenzylamine, 22.3g of sodium hydroxide, 42.5g of carbon disulfide, 69.5g of 50% sulfuric acid, 47.9g of 27% hydrogen peroxide solution, and 600g of water;

[0033] 2. Add dibenzylamine and sodium hydroxide into 200g of water according to the proportion, add carbon disulfide dropwise at a rate of 9ml / min at room temperature, cool down to 0°C after dropping, filter and separate the precipitated solid;

[0034] 3. Put the obtained solid into a new reaction vessel, add 360g of water to dissolve it, and then lower the temperature to 10°C.

[0035] 4. Add 50wt% sulfuric acid dropwise to the reaction vessel in step 3 at a rate of 25ml / min, control the reaction temperature during and after the dropwise addition to be 10°C, and then add 27wt% hydrogen peroxide solution at a rate of 1ml / min Continue to add dropwise into the reaction vessel at a speed of 1 min, and control the reaction temperature during the dropwise addition to 10°C. After dr...

Embodiment 2

[0038] 1. Weigh each raw material: 100g of dibenzylamine, 20.3g of sodium hydroxide, 38.6g of carbon disulfide, 49.7g of 50% sulfuric acid, 31.9g of 27% hydrogen peroxide solution;

[0039] 2. Add dibenzylamine and sodium hydroxide to the filtrate of step 2 in Example 1 according to the proportioning ratio. If the filtrate is less than 200g, make up with pure water. Add carbon disulfide dropwise at a rate of 9ml / min at normal temperature, drop After cooling down to 0°C, filter and separate the precipitated solid;

[0040] 3. Put the obtained solid into a new reaction vessel, add the filtrate from Step 4 in Example 1, make up for the filtrate less than 360g with pure water, stir to dissolve, and then lower the temperature to 10°C.

[0041] 4. Add 50wt% sulfuric acid dropwise to the reaction vessel in step 3 at a rate of 25ml / min, control the reaction temperature during and after the dropwise addition to be 10°C, and then add 27wt% hydrogen peroxide solution at a rate of 1ml / min...

Embodiment 3

[0043] 1. Weigh each raw material: 100g of dibenzylamine, 20.3g of sodium hydroxide, 38.6g of carbon disulfide, 49.7g of 50% sulfuric acid, 31.9g of 27% hydrogen peroxide solution;

[0044] 2. Add dibenzylamine and sodium hydroxide into the filtrate of step 2 in Example 2 according to the proportioning ratio. If the filtrate is less than 200g, make up with pure water. Add carbon disulfide dropwise at a rate of 10ml / min at normal temperature, drop After cooling down to 0°C, filter and separate the precipitated solid;

[0045] 3. Put the obtained solid into a new reaction vessel, add the filtrate from Step 4 in Example 2, make up the filtrate less than 360g with pure water, stir to dissolve, and then cool down to 8°C.

[0046] 4. Add 50wt% sulfuric acid dropwise to the reaction vessel in step 3 at a rate of 20ml / min, control the reaction temperature during and after the dropwise addition to be 8°C, then add 27wt% hydrogen peroxide solution at 2ml / min Continue to add dropwise in...

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Abstract

The invention discloses a clean production method of tetrabenzylthiuram disulfide. Reactions are carried out in two steps. Dibenzylamine, alkali and carbon disulfide are reacted to form an intermediate, the intermediate is separated out and added to a new reaction container for neutralization and oxidation, and mother solutions obtained in the two steps are reused in each step. The clean production method has the advantages that the condensation reaction and the oxidation reaction are carried out in two steps, the mother solutions generated in each step are recycled, no waste water and waste residues are generated, the pollution is small, energy conservation and environmental protection are achieved, the production cost is reduced, the process safety hazards are reduced, the product yield is high, and the clean production method is adaptable to national policy requirements for green chemical engineering.

Description

technical field [0001] The invention relates to a production method of tetrabenzylthiuram disulfide, in particular to a low-cost, clean and environment-friendly method for producing tetrabenzylthiuram disulfide, which belongs to the technical field of fine chemicals. Background technique [0002] Rubber accelerator Tetrabenzylthiuram disulfide (TBzTD) is a new, safe and environmentally friendly thiuram accelerator. TBzTD is a safe secondary amine-based accelerator without nitrosamine hazards. Its high relative molecular weight and performance are incomparable to low relative molecular weight thiurams. The main features of this product are: (1) The vulcanization acceleration effect is equivalent to TMTD, the vulcanization speed is slightly slower than TMTD, but the stability is better than TMTD; (2) It will not produce carcinogenic nitrosamines, it is a green, A safe, environmentally friendly and efficient vulcanization accelerator that can replace TMTD, TETD, and MPhTD; (3)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/32
CPCC07C333/32
Inventor 孟祥克马德龙王才朋徐思明黄存影王克军崔亭亭张尊政
Owner SHANDONG YANGGU HUATAI CHEM
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