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CTP synthesis technology of rubber scorch retarder and device thereof

A technology of anti-scorching agent and rubber, which is applied in the field of rubber anti-scorching agent CTP synthesis process, can solve the problems of unstable cyclohexylsulfenyl chloride, affecting the efficiency of reaction, and long time required for mixing, so as to reduce the chance of decomposition , Promote mixing and improve yield

Active Publication Date: 2011-09-21
SHANDONG YANGGU HUATAI CHEM
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The common feature of the above-mentioned preparation methods is that the reaction process includes chlorination, condensation, crystallization, filtration and drying, wherein the condensation reaction is to mix the two materials in the reactor, and this method will make part of the phthalimide Wrapped by the generated CTP, affecting the efficiency of the reaction
In addition, the time required for mixing is long, cyclohexylsulfanyl chloride is unstable, and the reaction yield is low

Method used

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  • CTP synthesis technology of rubber scorch retarder and device thereof
  • CTP synthesis technology of rubber scorch retarder and device thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: tubular reactor

[0024] The tubular reactor structure is as figure 1 shown. The size of the cylindrical chamber 13 is φ200mm×800mm. Two material feeding pipes 1, 2 and a nitrogen gas inlet pipe 3 are passed into the chamber from the upper side outside the chamber. The three pipes merge and communicate with a mixing vertical pipe 4. Material standpipe 4 is long 30mm. The nitrogen inlet pipe 3 is located at the center between the two material feeding pipes 1 and 2, and the two material feeding pipes 1 and 2 are arranged symmetrically. A funnel-shaped mixing pipe 7 is arranged at the center of the lower part of the chamber, and the length of the funnel-shaped mixing pipe 7 is 80 mm. The outer wall of the cavity is provided with a thermal insulation jacket 5, and the thermal insulation jacket 5 is provided with thermal insulation medium inlets and outlets 9, 11. There is a material outlet 10 at the bottom of the cavity directly leading to the condensation...

Embodiment 2

[0025] Embodiment 2: Synthesis of rubber anti-scorch agent CTP

[0026] (1) prepare cyclohexyl sulfenyl chloride with chlorine, dicyclohexyl disulfide and organic solvent in a reaction still (also become chlorination still) according to prior art, simultaneously in another reaction still, use phthalo Phthalimide sodium salt was prepared from imide and sodium hydroxide solution.

[0027] (2) Feed nitrogen into the tubular reactor for 4min to replace the mixture of organic solvent vapor and air inside. The tubular reactor size is φ 200mm × 600mm, and its structure is as described in Example 1. In the insulation jacket 5 The insulation medium used is ethylene glycol.

[0028] (3) then the cyclohexylsulfenyl chloride prepared by above-mentioned steps (1) and phthalimide sodium salt are continuously added in the tubular reactor by two material feeding pipes respectively with 1: 1 molar ratio, The feed rate is controlled to be 75-90 mol / min. The reaction temperature is 0-5°C, and...

Embodiment 3

[0032] Embodiment 3: rubber anti-scorch agent CTP is synthesized, as described in embodiment 2, difference is:

[0033] Cyclohexylsulfanyl chloride and phthalimide sodium salt are continuously added to the tubular reactor through two material feed pipes at a molar ratio of 1:1.1, and the heat preservation medium used in the heat preservation jacket 5 is ethanol , the reaction temperature is -5 ~ 3 ° C, and nitrogen is continuously fed, and the pressure is controlled at 0.2 ~ 0.3Mpa. After the first reaction in the tubular reactor, the material reacted for 50 minutes under stirring at 5-10°C in the condensation kettle to obtain a mixture of rubber anti-scorch agent CTP, organic solvent and water, and then through water separation, crystallization, and pressure filtration and drying to obtain the finished rubber anti-scorch agent CTP. The CTP purity of the obtained rubber anti-scorch agent is increased from 96.6% in the existing traditional process to 98.5%, and the product yie...

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Abstract

The invention relates to a CTP synthesis technology of rubber scorch retarder and a device thereof. The technology comprises the following steps of: continuously adding cyclohexyl sulfenyl chloride and phthalimide sodium salt into a tube type reactor, continually adding with nitrogen, momentary completely mixing the cyclohexyl sulfenyl chloride and the phthalimide sodium salt at the tube type reactor and reacting, adding materials into a condensation kettle, and continuously stirring to have a condensation reaction under consistent temperature. The invention also provides a special tube type reactor. By adding a pipeline condensation reaction, the invention can reduce the decomposition probability of the cyclohexyl sulfenyl chloride, thereby heightening yield efficiency to be more than 92% and purity to be more than 98%.

Description

technical field [0001] The invention relates to a synthesis process of a rubber antiscorch agent CTP (N-cyclohexylthiophthalimide), which belongs to the field of fine chemicals. Background technique [0002] The chemical name of rubber anti-scorch agent CTP is N-cyclohexylthiophthalimide, which is widely used in elastomers that can be vulcanized by sulfur. It has a good anti-scorch effect when used in combination with various general-purpose accelerators. See CN1059906A cyclohexyl Preparation of N-cyclohexylthiophthalimide by alkane chlorination method is part of background technology. Whether it is open or high-temperature rapid mixing with CTP, one-stage mixing process can be used to effectively prevent early vulcanization (scorch) of the rubber during operation, and at the same time it does not hinder the normal performance of the vulcanization accelerator, which can realize rubber production The sealed mixing of medium rubber can increase the preheating temperature when...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48B01J19/24C08K5/3417
Inventor 王文博王传华杜孟成许思俊郑崇纳
Owner SHANDONG YANGGU HUATAI CHEM
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