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Green preparation method of isothiocyanate compounds

A technology of isothiocyanate and compounds, which is applied in the field of green preparation of isothiocyanate compounds, can solve the problems of difficult solid waste treatment, incomplete dissolution, and reduced product content, so as to avoid post-processing work, low cost, and easy The effect of treatment

Active Publication Date: 2019-11-26
湖北中迅长青科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The conventional method for recovering thiocyanate in wastewater is to directly add a certain amount of thiocyanate to the wastewater to continue the next batch reaction, but this will lead to too much total salt in the system, which cannot be completely dissolved and affects the reaction; The enrichment of impurities leads to lower product content; finally, solids of mixed salts (thiocyanate and halogenated salts) will appear in the wastewater, causing solid waste treatment problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Install a stirrer, a reflux condenser, and a thermometer on a 1000mL four-necked reaction flask, add 496g (1.2mol) 20% sodium thiocyanate aqueous solution and 0.3g N,N-dimethyl-4-aminopyridine into the four-necked flask for 4 hours 77.3g of 3-chloropropene (1.0mol) was added dropwise at 60°C, and the reaction was kept for 1 hour after the dropwise addition. After standing still, the phases were separated, and the organic phase was 100 g (99.2%) of 3-isothiocyanatopropyl-1-ene, with a yield of 99.1% (calculated as 3-chloropropene). The water phase was added to the flask, and 77.3g of 3-chloropropene (1.0mol) was added dropwise at 60°C within 2 hours, and the phases were separated after standing. The organic phase was a mixture of 3-isothiocyanatopropyl-1-ene and chloropropene 81.5 g, the concentration of thiocyanate in the wastewater is 4ppm, and the COD is 1814mg / L. Then add 413g (1.0mol) 20% sodium thiocyanate aqueous solution and 0.3g N,N-dimethyl-4-aminopyridine int...

Embodiment 2

[0031] Install a stirrer, a reflux condenser, and a thermometer on a 1000mL four-necked reaction flask, add 356g (1.1mol) 20% potassium thiocyanate aqueous solution and 0.2g N,N-dimethyl-4-aminopyridine into the four-necked flask for 4 hours 138.5 g of bromobutane (1.0 mol) was added dropwise at 98°C, and the reaction was kept for 1 hour after the dropwise addition was completed. After standing still, the phases were separated, and the organic phase was 115.9 g (98.8%) of 1-isothiocyanatobutane, with a yield of 99.5% (calculated as bromobutane). Add the water phase to the flask, add 138.5g bromobutane (1.0mol) dropwise at 98°C within 2 hours, stand still and separate the phases, the organic phase is a mixture of 1-isothiocyanatobutane and bromobutane 136.2g, in the waste water Thiocyanate concentration 5ppm, COD 1927mg / L. Then add 323.7g (1.0mol) 20% aqueous solution of potassium thiocyanate and 0.2g N,N-dimethyl-4-aminopyridine into the four-necked flask, and dropwise add th...

Embodiment 3

[0033] Install a stirrer, a reflux condenser, and a thermometer on a 1000mL four-necked reaction flask, add 456g (1.2mol) 20% ammonium thiocyanate aqueous solution and 0.3g N,N-dimethyl-4-aminopyridine to the four-necked flask for 4 hours 122.3g of 3-bromopropene (1.0mol) was added dropwise at 50°C, and the reaction was kept for 1 hour after the dropwise addition. After standing still, the phases were separated, and the organic phase was 99.2 g (99.0%) of 3-isothiocyanatopropyl-1-ene, with a yield of 99.2% (calculated as 3-bromopropene). Add the water phase to the flask, add 122.3g of 3-bromopropene (1.0mol) dropwise at 50°C within 2 hours, let stand to separate the phases, and the organic phase is a mixture of 3-isothiocyanatopropyl-1-ene and 3-bromopropene Mixture 117.0g, concentration of thiocyanate in wastewater 2ppm, COD 1991mg / L. Then add 380g (1.0mol) 20% ammonium thiocyanate aqueous solution and 0.3g N,N-dimethyl-4-aminopyridine into the four-necked flask, and dropwis...

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Abstract

The invention discloses a green preparation method of isothiocyanate compounds. The method comprises the following steps: step 1, performing a reaction on first batch of added materials: dissolving athiocyanate into water, adding a catalyst, adding an organic halide dropwise, performing a condensation reaction, and after the reaction is completed, allowing the reaction products to stand for phaseseparation to obtain an isothiocyanate compound organic phase and a first aqueous phase, wherein the molar ratio of the amount of the thiocyanate to the organic halide in the step 1 is (1.1-1.3):1. The method provided by the invention has the following beneficial effect: 1, the method changes a traditional reaction mode which adopts excess organic halide (requiring rectification recovery) or excess thiocyanate (requiring complicated wastewater treatment), and achieves the goal of organic combination of excessive reaction materials in local stages and non-excessive reaction materials in the whole process.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a green preparation method of isothiocyanate compounds. Background technique [0002] Isothiocyanate compounds are an important class of fine chemical intermediates. Due to their high reactivity, they are used to synthesize a variety of heterocyclic compounds containing nitrogen, sulfur, and oxygen. It has important biological activities such as antibacterial, anti-inflammatory and anti-cancer in medicine; it can be used as bactericide, herbicide and insecticide in agriculture; it is also used to determine the amino acid sequence and fluorescein marker in peptides and proteins. The chemical structure of isothiocyanate compounds is shown in general formula (I): [0003] (I) [0004] At present, the most simple and low-cost industrial method of isothiocyanate is to use organic halides and thiocyanate as raw materials, and react them in aqueous phase. [0005] [...

Claims

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Application Information

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IPC IPC(8): C07C331/22C07C331/20
CPCC07C331/20C07C331/22
Inventor 王宇周灿亮杨彬
Owner 湖北中迅长青科技有限公司
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