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Method for preparing 1,1,3,3-tetramethyl thiourea

A technology of tetramethylthiourea and dimethylformamide, applied in the first field, can solve the problems of high raw material cost, toxicity, safety hazards, etc., and achieve the effect of low cost and simple operation

Inactive Publication Date: 2012-07-11
ZHEJIANG UNIV
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  • Claims
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Problems solved by technology

There is a common defect in the above several methods: raw material cost is higher, in addition, sulfur oxychloride and dimethylamine are all toxic chemicals, there is a safety hazard in the production process of synthesizing tetramethylthiourea as raw material with this Hidden danger

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  • Method for preparing 1,1,3,3-tetramethyl thiourea

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Embodiment 1

[0008] Embodiment 1: 1,1,3, the preparation method of 3-tetramethylthiourea, carry out following steps successively:

[0009] Add 3.2g (0.1mol) of sulfur and 30g (about 0.4mol) of DMF to the reactor, heat until the sulfur is completely dissolved, add 3.5g (about 0.15mol) of sodium, and heat up to 120°C for 2 hours to complete the reaction. The reaction liquid was distilled, and fractions of components at 243-246°C were collected to obtain 8.5 g of 1,1,3,3-tetramethylthiourea (purity: 99%), with a yield of 64%.

Embodiment 2～5

[0011] 1,1,3, the preparation method of 3-tetramethylthiourea, change the following reaction conditions among the embodiment 1: DMF consumption (abbreviation R1), sodium consumption (abbreviation R2), reaction time (abbreviation t), temperature of reaction (abbreviation T), thereby correspondingly obtaining embodiment 2~5,1,1,3, the yield of 3-tetramethylthiourea is Y and purity etc. and specific content and data result are shown in Table 1.

[0012] Table 1

[0013] Example 2 3 4 5 R1, g 25 30 25 20 R2, g 3 3.5 2.5 3 t, h 4 5 3 3.5 T，℃ 120 140 110 130 Y，％ 68 79 61 72 purity,% 99 99 99 99

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Abstract

The invention discloses a method for preparing 1,1,3,3-tetramethyl thiourea, comprising the steps of subjecting N,N-dimethyl formamide (DFM), sulfur and sodium to reaction for 6 hours at 100-150 DEG C, and distilling a solution of reaction to obtain the 1,1,3,3-tetramethyl thiourea, wherein the molar ratio of the sulfur to the DFM to the sodium is 1:(1-8):(1-3). The method for preparing the 1,1,3,3-tetramethyl thiourea has the characteristics of simple operation and low cost.

Description

technical field [0001] The invention relates to a preparation method of 1,1,3,3-tetramethylthiourea. Background technique [0002] 1,1,3,3-tetramethylthiourea as shown in formula I is a rubber overspeed vulcanization accelerator, suitable for natural rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, and EPDM Rubber, mainly used as an accelerator for modified acrylate adhesives. There are three main synthetic methods of tetramethylthiourea: it is reported that tetramethylthiourea is synthesized by reacting thiourea with methyl iodide (Synthesis, 1984, 2, 136); Tetramethylthiourea (Russian Journal of General Chemistry, 2008, 78(7): 1341-1344); Another method is to react with thionyl chloride and dimethylamine to generate tetramethylsulfur after removing two molecules of hydrogen chloride Urea (Bulletin de la Societe Chimique de France, 1910, 7(4):993). There is a common defect in the above several methods: raw material cost is higher, in addition, sulfur oxy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/08
Inventor 陈新志周少东钱超
Owner ZHEJIANG UNIV
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