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
View PDF3 Cites 1 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Green preparation method of isothiocyanate compounds
  • Green preparation method of isothiocyanate compounds

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0028]

[0029] Install a stirrer, reflux condenser, and thermometer on a 1000mL four-necked reaction flask, add 496g (1.2mol) 20% sodium thiocyanate aqueous solution and 0.3gN,N-dimethyl-4-aminopyridine to the four-necked flask for 4h 77.3g of 3-chloropropene (1.0mol) was added dropwise at 60°C, and the temperature keeping reaction was completed for 1h. Let stand for phase separation, the organic phase is 100 g (99.2%) of 3-isothiocyanopropyl-1-ene, and the yield is 99.1% (based on 3-chloropropene). The water phase was added to the flask, and 77.3g 3-chloropropene (1.0 mol) was added dropwise at 60°C within 2 hours, and the phases were separated. The organic phase was a mixture of 3-isothiocyanopropyl-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 into the four-necked flask, add dropwise the isothiocyanate o...

Example Embodiment

[0030]

[0031] Install a stirrer, reflux condenser, and thermometer on a 1000mL four-necked reaction flask. Add 356g (1.1mol) 20% potassium thiocyanate aqueous solution and 0.2gN,N-dimethyl-4-aminopyridine to the four-necked flask for 4h 138.5g bromobutane (1.0mol) was added dropwise at 98°C, and the temperature keeping reaction was completed for 1h. Let stand for phase separation, the organic phase is 115.9 g (98.8%) of 1-isothiocyanobutane, with a yield of 99.5% (calculated as bromobutane). The water phase was added to the flask, and 138.5g of bromobutane (1.0mol) was added dropwise within 2h at 98°C, and the phases were separated. The organic phase was a mixture of 1-isothiocyanatobutane and bromobutane, 136.2g, in the wastewater The concentration of thiocyanate is 5ppm and COD is 1927mg / L. Then 323.7g (1.0mol) 20% potassium thiocyanate aqueous solution and 0.2g N,N-dimethyl-4-aminopyridine were added to the four-neck flask, and the 1- 136.2g of a mixture of isothiocyanob...

Example Embodiment

[0032]

[0033] Install a stirrer, reflux condenser, and thermometer on a 1000mL four-necked reaction flask. Add 456g (1.2mol) 20% ammonium thiocyanate aqueous solution and 0.3gN,N-dimethyl-4-aminopyridine to the four-necked flask for 4h Add 122.3g of 3-bromopropene (1.0 mol) dropwise at 50°C, and complete the heat preservation reaction for 1 hour. Let stand for phase separation, the organic phase is 99.2 g (99.0%) of 3-isothiocyanopropyl-1-ene, and the yield is 99.2% (based on 3-bromopropene). The water phase was added to the flask, 122.3g of 3-bromopropene (1.0mol) was added dropwise at 50°C within 2h, and the phases were separated. The organic phase was composed of 3-isothiocyanopropyl-1-ene and 3-bromopropene. The mixture is 117.0g, the thiocyanate concentration in the wastewater is 2ppm, and the COD is 1991mg / L. Then add 380g (1.0mol) 20% ammonium thiocyanate aqueous solution and 0.3g N,N-dimethyl-4-aminopyridine into a four-necked flask, and add dropwise the 3-isopropion...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products