Synthetic process of N-allyl-O- isobutyl thionocarbamate

A synthesis process, allyl technology, applied in the direction of organic chemistry, etc., can solve the problems of low content of allyl isobutyl thiourethane, low conversion rate, etc., and achieve strong reaction activity, improved environmental conditions, and residual amount. reduced effect

Active Publication Date: 2015-11-18
SHENYANG YOUYAN MINERAL CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problems of low content and low conversion rate of allyl isobutyl thiocarbamat

Method used

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  • Synthetic process of N-allyl-O- isobutyl thionocarbamate
  • Synthetic process of N-allyl-O- isobutyl thionocarbamate
  • Synthetic process of N-allyl-O- isobutyl thionocarbamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 0.25 moles of allyl isothiocyanate and 0.5 moles of isobutanol are co-heated to 110°C under normal pressure, and catalyzed by 0.4 g / mole of trimethylchlorosilane or tetrabutyl titanate. The reaction was carried out accordingly, and the conversion was determined by gas chromatography. The reaction results are shown in Table 1:

[0021]

[0022] The data in Table 1 shows that using trimethylchlorosilane as a catalyst compared with tetrabutyl titanate or iron acetylacetonate as a catalyst, the conversion rate has been greatly improved after 3-6 hours of reaction.

Embodiment

[0024] Carry out the reaction according to Experiment 1, and change the molar ratio of reaction with isobutanol to 1:1, and the test results are shown in Table 2:

[0025]

[0026] The data given in Table 2 shows that when the molar ratio of the reaction with isobutanol is 1:1, using trimethylchlorosilane as the catalyst, the conversion rate and purity of this reaction are relatively high in a short period of time.

Embodiment 3

[0028] The reaction of allylthiocarbamate with propanol

[0029] Except that 0.25 mol of isobutanol was replaced by 0.25 mol of propanol, the experimental procedure was the same as that of experiment 2. Use 0.1 g trimethylchlorosilyl ester (0.4 g / mol allyl thiocyanate). Heating at 110°C for 6 hours yielded N-allyl-O-propyl-thiocarbamate with a conversion rate of 97.2% and a purity of 89.8%.

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Abstract

The invention relates to the field of synthesis of chemical products and production of beneficiation reagents, in particular to a synthetic process of N-allyl-O- isobutyl thionocarbamate. The synthetic process is characterized in that the use quantity of a catalyst in a reaction is about 0.5-4 mole percent while the general use quantity of the catalyst is between 0.1 mole percent to 1 mole percent; the production technology improves the appearance, the yield and the odor of an N-allyl-O- isobutyl-thiocarbamate product prepared with fatty alcohol; an initial reactant allyl isothiocyanate is prepared through a reaction of allyl halide and alkali metal or ammonium thiocyanate under the action of a phase transfer catalyst; then the fatty alcohol, the catalyst prepared in the process and trimethylchlorosilane are added for the reaction; a reaction mixture is heated to 100-120 DEG C, and heat preservation is performed for 3-6 h. When the reaction is ended, unreacted alcohol is pumped through vacuum, and trimethylchlorosilane serving as the synthetic catalyst has higher reactivity, so that the reaction conversion rate is increased.

Description

technical field [0001] The invention relates to the fields of chemical product synthesis and ore dressing agent production, in particular to a synthesis process of N-allyl-O-isobutylthiocarbamate. Background technique [0002] Allyl isobutyl thiocarbamate, scientific name N-allyl-O-isobutyl-thiocarbamate, also known as PAC in China, is a new type of mineral processing collector, its dosage is small, It has strong collection ability and good selectivity; it can improve the grade of copper concentrate and the recovery rate of copper and gold. It is an excellent collection accelerator for the separation of metal sulfide ores such as copper and zinc. One of the polluted environment-friendly ester beneficiation agents. [0003] At present, there are many studies on allyl isothiocyanate in China. Yu Yueqin, Kang Congmin, Li Zhijun, Wang Hao and others have discussed the synthesis of allyl isothiocyanate by many researchers; American cyanamide company applied for patent protectio...

Claims

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Application Information

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IPC IPC(8): C07C333/04
Inventor 王咏梅张海龙牟松郭靖宇汪世跃
Owner SHENYANG YOUYAN MINERAL CHEM CO LTD
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