CN105085333B - The preparation method of first sulfanilamide (SN) - Google Patents
The preparation method of first sulfanilamide (SN) Download PDFInfo
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- CN105085333B CN105085333B CN201510481050.0A CN201510481050A CN105085333B CN 105085333 B CN105085333 B CN 105085333B CN 201510481050 A CN201510481050 A CN 201510481050A CN 105085333 B CN105085333 B CN 105085333B
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Abstract
The present invention relates to the preparation method of first sulfanilamide (SN), specific steps include：Diazo reaction, displacement reaction, chlorination reaction, standing reaction, aminating reaction, neutralization reaction, dehydration, drying, packaging.Wherein dehydration be mother liquor is placed in diaphragm pressing filter extruded, eardrum squeezing, extruded again after washing, eardrum, by traditional centrifugal dehydration isolation technics, it is filter-press dehydration isolation technics to initiate, and reaches the purpose of dehydration.This method is more economized on electricity compared with prior art, water saving, and the production capacity under equal energy consumption greatly improved, while improving production environment, reduces labour intensity.
Description
Technical field
The present invention relates to a kind of preparation method of first sulfanilamide (SN).
Background technology
O-methyl formate benzene sulfonamide abbreviation first sulfanilamide (SN), CAS numberings：57683-71-3, is insoluble in water, be dissolved in alcohol, ether,
The white solid of the organic solvents such as benzene.As medicine, pesticide intermediate, it is mainly used in the synthesis of sulfonylurea herbicide, is to remove
The intermediate of careless agent metsulfuron-methyl, Sulfometuron Methyl and ethametsulfuron.At present, first sulfanilamide (SN) is removed as efficient, wide spectrum, low toxicity and high selectivity
The intermediate of careless agent, is used by numerous production herbicide producers.
First sulfanilamide (SN) production technology mainly has two kinds, respectively neighbour's formyl benzenesulfonimide esterification process (abbreviation saccharin method) and neighbour
Methyl formate benzene sulfonyl chloride amination method.It is anti-that the technological process of o-methyl formate benzene sulfonyl chloride production first sulfanilamide (SN) generally includes diazonium
Reaction, chlorination reaction, should be replaced, reaction, aminating reaction, neutralization reaction, dehydration, drying, packaging etc. is stood.In traditional handicraft
Dehydration is that mother liquid obtained being placed in geosyncline of previous step is carried out into vacuum filtration (pumping a hypo acid), adds water washing suction filtration again,
Reactor so is squeezed into pump after 8-9 time repeatedly, adding 25-30%H2O2 react 45 minutes, then blowing is to filter pocket
Suction filtration, carries out drying of drawing water again again after the completion of suction filtration.This kind of method water consumption is big, efficiency is low, is unfavorable for economical environment-protective.For with
Upper problem, changing the mode being dehydrated in traditional o-methyl formate benzene sulfonyl chloride amination method just becomes necessary.
The content of the invention
It is an object of the present invention to be dehydrated water consumption in overcoming o-methyl formate benzene sulfonyl chloride amination method in the prior art
Greatly, the low deficiency of efficiency, there is provided a kind of method of new dehydration, the method step is relatively easy, is suitable to practicality.
The purpose of the present invention and the technical problem of solution are realized using following technical scheme.The invention provides
A kind of preparation method of first sulfanilamide (SN), comprises the following steps：Diazo reaction, displacement reaction, chlorination reaction, standing reaction, amination are anti-
Should, neutralization reaction, dehydration, drying, packaging, it is characterised in that the dehydration using following steps complete：
(1) squeezing into the mother liquor high-pressure pump obtained after neutralization reaction step makes diaphragm pressing mistake in diaphragm pressing filter
Filter pressure reaches 0.6Mpa, and diaphragm pressing filter carries out first time extruding, extrudes the mother liquor sour water of 75-78%, Ran Houjin
Row eardrum is squeezed.
(2) adding the water of amount of solid 10% carries out secondary washing, when intake pressure reaches 0.4Mpa, carries out secondary squeezing
Pressure, and secondary tympanic membrane again, make mother liquor PH reach 6, ammonia-nitrogen content≤0.002%.
(3) carried out reciprocation cycle 5-10 minutes to the H2O2 that 25% is added in mother liquor by high-pressure pump, after circulation is finished,
Extruding eardrum is carried out again, obtains finished product of the moisture content less than 15%.
Diaphragm pressing filtering machine structure is solid slab mutually arranged with hollow, and eardrum refers to that diaphragm pressing filter is carried
High-pressure pump adds water to cored slab makes its pressure reach 1.2Mpa, cored slab is expanded the effect for reaching extruding.
The object of the invention to solve the technical problems can also be applied to the following technical measures to achieve further.
The preparation method of foregoing first sulfanilamide (SN), wherein 160 meters described of the high pressure pump lift, flow 40t/h.
By above-mentioned technical proposal, the present invention at least has following advantages：
(1), by traditional centrifugal dehydration isolation technics, it is secondary filter-press dehydration isolation technics to initiate.
(2) power consumption is 17.5 kilowatts of 55 kilowatts of ratios, economize on electricity 96.8% to this technology compared with prior art.Prior art is to stir
Washing is mixed, this technology is washed for infiltration, water consumption is 100 tons of 70 tons of ratios, water saving 30%.Equal energy consumption production capacity improves 65%.
(3) prior art dehydration is completed in two times, and this technology dehydration washing is one in the production of adjacent sulfonamide benzoic acid methyl esters
Secondary completion, reduces labour intensity and device configuration diversity.
(4) prior art centrifugal dehydration safety is uncontrollable with acid mist environment, and the hermetically sealed dehydration of this technology is washed and discharged,
Prevent safe operation hidden danger and environmental pollution, improve production environment and reduce operation labour intensity.
In sum, the present invention has the advantages that many and practical value, and there are no similar design publish or
Using and really belong to innovation, it is technically had large improvement, and generates the effect of practicality, and the extensive utilization with industry
Value, is really a new and innovative, progressive, practical new design.
Described above is only the general introduction of technical solution of the present invention, in order to better understand technological means of the invention,
And can be practiced according to the content of specification, described in detail as after with presently preferred embodiments of the present invention below.
Concrete operation method of the invention is shown in detail by following examples.
Brief description of the drawings
Fig. 1 is o-methyl formate benzene sulfonyl chloride production first sulfanilamide (SN) preparation method schematic flow sheet；
Fig. 2 is gained finished product infrared spectrogram；
Fig. 3 is first sulfanilamide (SN) standard items infrared spectrogram；
Fig. 4 is gained finished product HPLC spectrograms；
Fig. 5 is first sulfanilamide (SN) standard items HPLC spectrograms.
Specific embodiment
In order that the technical problem to be solved, technical scheme and beneficial effect become more apparent, with reference to embodiments,
The present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain this hair
It is bright, it is not intended to limit the present invention.
The concrete technology step of production method of the present invention is as follows：
(1) using the method for traditional o-methyl formate benzene sulfonyl chloride production first sulfanilamide (SN) raw material is carried out successively diazo reaction,
The steps such as displacement reaction, chlorination reaction, standing reaction, aminating reaction, neutralization reaction.
Fig. 1 display o-methyl formate benzene sulfonyl chloride production first sulfanilamide (SN) technological processes.Now configured by water, hydrochloric acid, sulfuric acid
Nitration mixture be placed in diazonium pot, slow plus methyl anthranilate (abbreviation methyl esters) is started after cooling mixed with sodium nitrite solution
Liquid is closed, diazonium temperature is maintained at less than 25 DEG C, and reaction end shows lavender with starch potassium iodide solution.Diazo liquid is cooled to 10
DEG C, add copper sulphate, logical sulfur dioxide to enter line replacement, separate out adjacent sulfinic acid methyl benzoate.Toluene is subsequently adding, leads to chlorine chlorine
Change, it is terminal to show deeply blackish green with the test of 2% benzidine ethanol solution.Stratification, organic layer is adjacent methyl formate benzene sulfonyl
Chloromethane benzole soln.O-methyl formate benzene sulfonyl chloride is put into ammoniation kettle, liquefied ammonia is passed through at 10 DEG C, keep 15 DEG C of humidity, reaction 5 is small
When, filtered after stratification.Use acetic acid pickling.
(2) 2 350 squares of diaphragm pressing filter is configured, it is ensured that the 4T of diaphragm pressing filter discharging per hour.Will be anti-
The mother liquor input diaphragm pressing filter that neutralization reaction in kettle is obtained is answered, the separation of solid and liquid of mother liquor is realized.When diaphragm pressing filtering
Machine operating pressure is 0.6MPa, when the liquid outlet quantity of liquid outlet is reduced or do not go out liquid, is illustrated in diaphragm pressing filter sheet frame volume
Solid material is had been filled with, now stops conveying.Start diaphragm plate high-pressure pump, hydraulic pressure is reached 1.2-1.6MPa, carry out eardrum squeezing.
Mother liquor flows into mother liquor collecting pit.
(3) washings of solid doses 10% are input into diaphragm filter press, carry out the washing of solid material.After completing washing,
Extruding and the eardrum of previous step are repeated, the acid of removal 1% makes mother liquor PH reach 6, ammonia-nitrogen content≤0.002%.
(4) carried out reciprocation cycle 5-10 minutes to the H2O2 that 25% is added in mother liquor by high-pressure pump, it is therefore an objective to remove material
A small amount of ammonia nitrogen and COD in liquid.After circulation is finished, then extruding eardrum is carried out, obtain finished product of the moisture content less than 15%.
(5) by packaging and storage after finished product drying.
2 diaphragm pressing filters always feed 12T, and filtering-washing-filtering a cycle time is set as 3 hours, produces
During according to product actual effect, the work period can adjust accordingly.
Scene needs configuration：2 diaphragm pressing filters, the feed pump of 40T/H, the high-pressure hydraulic pump that 160 meters of lift, 3 receipts
Liquid pool, 3 discharging belt conveyor pipelines and valve are some.
The infrared spectrogram of Fig. 2 display gained finished products, Fig. 3 shows the infrared spectrogram of first sulfanilamide (SN) standard items.Contrast two is composed
Figure, it may be determined that gained finished product is first sulfanilamide (SN).
The HPLC spectrograms of Fig. 4 display gained finished products, Fig. 5 display first sulfanilamide (SN) standard items HPLC spectrograms.HPLC spectrogram results are said
It is bright：Finished product is consistent with standard items retention time；Area normalization method measures finished product purity and is not less than 98.5%, reaches as high as
99.6%, standard items result is 98%.
Claims (1)
1. a kind of preparation method of first sulfanilamide (SN), comprises the following steps：Diazo reaction, displacement reaction, chlorination reaction, stand react,
Aminating reaction, neutralization reaction, dehydration, drying, packaging, it is characterised in that the dehydration is completed using following steps：
(1) the mother liquor high-pressure pump obtained after neutralization reaction step is squeezed into diaphragm pressing filter, filters diaphragm pressing
Machine pressure reaches 0.6 MPa, and diaphragm pressing filter carries out first time extruding, mother liquor sour water is extruded 75-78%, Ran Houjin
Row eardrum is squeezed；Wherein described diaphragm pressing filtering machine structure is solid slab mutually arranged with cored slab；
(2) adding the water of amount of solid 10% carries out secondary washing, when intake pressure reaches 0.4 MPa, carries out secondary extrusion,
And secondary tympanic membrane again, mother liquor pH is reached 6, ammonia-nitrogen content≤0.002%；
(3) by high-pressure pump to the H that 25% is added in mother liquor2O2, carry out reciprocation cycle 5-10 minutes, after circulation is finished, then carry out
Extruding, eardrum, obtain finished product of the moisture content less than 15%；160 meters of wherein described high pressure pump lift, flow 40t/h.
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| CN108586381A (en) * | 2018-04-16 | 2018-09-28 | 天津北方食品有限公司 | A kind of preparation method of saccharin sodium |
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| CN100422162C (en) * | 2005-03-22 | 2008-10-01 | 天津北方食品有限公司 | Method for producing saccharin sodium |
| CN101130524B (en) * | 2006-08-23 | 2011-03-30 | 上海港福化工技术咨询有限公司 | Method for producing saccharin |
| CN102603582A (en) * | 2012-02-28 | 2012-07-25 | 王继龙 | Method for synthesizing o-methyl formate benzene sulfonamide |
| CN103709118B (en) * | 2013-12-19 | 2015-10-07 | 中国平煤神马集团开封兴化精细化工有限公司 | A kind of production method of soluble saccharin |
| CN104447423A (en) * | 2014-10-29 | 2015-03-25 | 湖北诺鑫生物科技有限公司 | Preparation process of methyl sulfonamide |
| CN204219818U (en) * | 2014-10-29 | 2015-03-25 | 湖北诺鑫生物科技有限公司 | Modified first sulfanilamide (SN) dehydration equipment |
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Effective date of registration: 20180301 Address after: 453600 Hongzhou industrial agglomeration area of Huixian City, Xinxiang, Henan Patentee after: Huixian moisten biological science and Technology Co., Ltd. Address before: 453600 Hongzhou Park, Hongzhou industrial agglomeration area, Xinxiang City, Henan Patentee before: XINXIANG HOPE CHEMICAL TECHNOLOGY CO., LTD. |
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