CN102816043A - Production method for sulfonyl isocyanate - Google Patents

Abstract

The invention provides a production method for sulfonyl isocyanate. The method comprises the steps of adding dimethylbenzene into a slurry-preparing kettle in one time; adding raw materials of sulfonamides to prepare a sulfanilamide slurry; cooling to a normal temperature for use; adding dimethylbenzene into a photochemical kettle as a base material; adding the sulfanilamide slurry and a catalyst into the photochemical kettle; passing phosgene through till to a reaction terminal point; transferring reaction product to a phosgene-driving kettle; driving phosgene with nitrogen; cooling to the normal temperature; filtering; and thus the product of sulfonyl isocyanate is obtained. The procedure simplifies a synthetic system of sulfonyl isocyanate, improves yield of sulfonyl isocyanate, simplifies operation programs and shortens reaction time. The whole process procedure is material balance and energy exchange balance. By controlling reaction conditions, high selectivity of the product is achieved; comprehensive utilization is reached; raw materials and energy consumption are decreased; and production cost is greatly reduced.

Description

The working method of sulfonylisocyanates

Technical field

The present invention relates to a kind of preparation method of chemical field, be specifically related to the working method of sulfonylisocyanates.

Background technology

Characteristics such as sulfonylisocyanates belongs to a kind of Chemicals, is widely used in industries such as medicine, agricultural chemicals, rubber manufacturing, and it has applied range, and result of use is good.Domestic present Urethylane ME is complicated, and the waste of raw materials rate is high, and product yield is low, and environmental pollution is serious, and to compare competitive power poor with external like product, can't satisfy that market is high-quality to this product, the demand of low price.

Summary of the invention

To the problem that exists in the above prior art, the invention provides the working method of the sulfonylisocyanates that a kind of technology is simple, utilization rate of raw materials is high, environmental pollution is little.

The present invention realizes through following technical scheme:

The working method of sulfonylisocyanates, said working method may further comprise the steps:

1) with in the disposable adding slurry of the YLENE configuration still, add the sulfonamides raw material and be configured to the sulfanilamide (SN) slurry, it is subsequent use to be cooled to normal temperature; Wherein the sulfonamides raw material is adjacent chlorobenzene sulfonamide, 2-sulfoamido-oil of Niobe, 2-Toluidrin yl benzoic acid methyl esters, 2-methoxycarbonyl-3-sulfonamido thiophene;

2) in photochemical still, add YLENE and do backing material; And material in the photochemical still is warming up to 110 ℃, and sulfanilamide (SN) slurry that obtains in the step 1 and catalyzer are added photochemical still, feed phosgene; The reinforced time of control be about three hours be that keeping photochemical still temperature of charge is 110-115 ℃; After treating that material dropping finishes, continue to feed phosgene until reaction end;

3) reaction product that obtains in the step 2 is transferred to catches up with the light still, catch up with light with nitrogen, postcooling to normal temperature promptly obtains the sulfonylisocyanates finished product after filtering.

Beneficial effect of the present invention is: process simplification of the present invention the synthetic system of sulfonylisocyanates, improved the productive rate of sulfonylisocyanates, simplified schedule of operation, shortened the reaction times.The material balance of whole process flow, energy exchange balance through the control of reaction conditions, have realized the highly selective of product, have reached rational comprehensive utilization, have reduced raw material and energy expenditure, have practiced thrift production cost greatly.

Embodiment

The present invention is configured to the sulfanilamide (SN) slurry with sulfonamides raw material (adjacent chlorobenzene sulfonamide, 2-sulfoamido-oil of Niobe, 2-Shen sulfamoylbenzoic acid methyl esters, 2-methoxycarbonyl-3-sulfonamido thiophene) and YLENE; The sulfanilamide (SN) slurry is that phosgene carries out under the effect of catalyzer photochemical synthetic; Catch up with light through nitrogen, get finished product after the filtration.

Concrete synthesis flow is: the YLENE that measures is disposed in the still with the disposable adding slurry of pump; Add the sulfonamides raw material that measures again; Sulphonamide is made into the sulfanilamide (SN) slurry, opens slurry still chuck water coolant import and export valve, it is subsequent use that material is cooled to normal temperature.Catalyzer after in the catalyzer scale tank, squeezing into metering is subsequent use.In photochemical still, add a certain amount of YLENE and do backing material, open photochemical synthesis reactor jacket steam import and export valve after finishing, material in the photochemical still is warming up to 110 ℃.

Open the slurry feed pump, catalyzer volume pump, phosgene under meter valve add photochemical synthesis reactor simultaneously in proportion with three kinds of materials, and the reinforced time of control is three hours, and photochemical still temperature of charge is 110-115 ℃.After treating that material dropping finishes, continue to feed phosgene reaction to terminal.Material is transferred to catches up with in the light still, light still temperature of charge is caught up with in control, catches up with light with nitrogen, material is transferred in the cooling reactor after the end again, and material is cooled to normal temperature, with pump material is transferred to storage tank through strainer again and at last finished product packing is sold.

Process simplification of the present invention the synthetic system of sulfonylisocyanates, improved the productive rate of sulfonylisocyanates, simplified schedule of operation, shortened the reaction times.The material balance of whole process flow, energy exchange balance through the control of reaction conditions, have realized the highly selective of product, have reached rational comprehensive utilization, have reduced raw material and energy expenditure, have practiced thrift production cost greatly.

Claims (1)

1. the working method of sulfonylisocyanates is characterized in that said working method may further comprise the steps:

1) with in the disposable adding slurry of the YLENE configuration still, add the sulfonamides raw material and be configured to the sulfanilamide (SN) slurry, it is subsequent use to be cooled to normal temperature; Wherein the sulfonamides raw material is adjacent chlorobenzene sulfonamide, 2-sulfoamido-oil of Niobe, 2-Toluidrin yl benzoic acid methyl esters, 2-methoxycarbonyl-3-sulfonamido thiophene;

2) in photochemical still, add YLENE and do backing material; And material in the photochemical still is warming up to 110 ℃, and sulfanilamide (SN) slurry that obtains in the step 1 and catalyzer are added photochemical still, feed phosgene; The reinforced time of control be about three hours be that keeping photochemical still temperature of charge is 110-115 ℃; After treating that material dropping finishes, continue to feed phosgene until reaction end;

3) reaction product that obtains in the step 2 is transferred to catches up with the light still, catch up with light with nitrogen, postcooling to normal temperature promptly obtains the sulfonylisocyanates finished product after filtering.