CN103709118A - Method for producing sodium saccharin - Google Patents
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- CN103709118A CN103709118A CN201310703050.1A CN201310703050A CN103709118A CN 103709118 A CN103709118 A CN 103709118A CN 201310703050 A CN201310703050 A CN 201310703050A CN 103709118 A CN103709118 A CN 103709118A
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- C07D275/00—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings
- C07D275/04—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings condensed with carbocyclic rings or ring systems
- C07D275/06—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings condensed with carbocyclic rings or ring systems with hetero atoms directly attached to the ring sulfur atom
Abstract
The invention discloses a method for producing sodium saccharin. The method comprises the following steps: with phthalic anhydride as a raw material, preparing a sodium saccharin solution with baume degree of 25-40 Be at 60 DEG C through an amidation reaction, an esterification reaction, a diazotization reaction, a substitution reaction, a chlorination reaction, an ammonolysis reaction and a neutralization reaction, decoloring, filtering, concentrating, crystallizing, centrifugally drying and drying to obtain a finished product of sodium saccharin, wherein the ammonolysis reaction comprises: with liquid ammonia as a raw material, reacting liquid ammonia with o-sulfonylchloride methylbenzoate obtained in the chlorination reaction to generate o-sulfonamide methylbenzoate. The production method can be used for shortening the process route, reducing the production procedures, lowering the production cost, as well as reducing the ammonia nitrogen emission in production wastewater, the emission of 1 moL NH4<+> can be reduced in each production of 1 moL sodium saccharin, so that the ammonia nitrogen emission in the production wastewater can be decreased by 50% to benefit environmental protection.
Description
Technical field
The present invention relates to the production method of a kind of production method of Chemicals, particularly a kind of soluble saccharin.
Background technology
Traditional soluble saccharin production technique is: take phthalic anhydride as raw material is through amidate action, esterification, doazo reaction, replacement(metathesis)reaction, chlorination reaction, aminating reaction, acid out, neutralization reaction, make soluble saccharin solution, this solution, through decolouring, concentrated, crystallization, drying, dry, is made to soluble saccharin finished product.Aminating reaction in traditional soluble saccharin production process is to take ammoniacal liquor as raw material, and the adjacent SULPHURYL CHLORIDE methyl benzoate obtaining with chlorination reaction reacts and generates saccharin ammonium.This production method not only production process route is long, and production link is many, and production cost is high, and the ammonia nitrogen quantity discharged in factory effluent is high.
Summary of the invention
The object of the present invention is to provide a kind of production method of soluble saccharin, it can reduce the ammonia in factory effluent, nitrogen discharged amount effectively, and can reduce production link, shortens operational path, can reduce production costs.
Production method of the present invention comprises following processing step:
1, amidate action: by mass concentration be about 16% ammoniacal liquor and water by phthalic anhydride with add ammoniacal liquor mass ratio be 1:0.1 proportional quantity is put into amidate action still, open stirring, air draft, condensation salt water for cooling, when temperature is down to 0 ℃ of left and right, the phthalic anhydride of the proportional quantity that to add by phthalic anhydride and ammoniacal liquor mass ratio be 1:0.1, adds phthalic anhydride, when temperature rises to 50-70 ℃, pH value is 7 o'clock, slowly adding mass concentration is the liquid caustic soda of 30% left and right, when pH value is 9, stops adding liquid caustic soda.The outlet temperature of amidate action, when 85 ℃ of left and right, is closed cooling salt solution, obtains qualified amidation liquid after insulation, ammonia excretion;
2, esterification: above-mentioned amidation liquid is squeezed in reaction kettle of the esterification, open stirring, open salt water for cooling, when temperature is down to 30 ℃, add phthalic anhydride and the add mass ratio of the methyl alcohol proportional quantity methyl alcohol that is 1:1.5, when temperature is down to below 10 ℃, add phthalic anhydride with add clorox mass ratio be the chlorine bleach liquor that 1:5 and mass concentration are 14%, add in chlorine bleach liquor's process, temperature of reaction must not surpass 30 ℃, with K1 reagent examination look, colour-fast in reaction process, esterification reaches terminal, stops adding chlorine bleach liquor.Close salt solution, when temperature rises to 40 ℃ of left and right, add the hot water of appropriate approximately 100 ℃, close and stir, static, after layering, upper strata methyl o-aminobenzoate is squeezed in methyl esters slurry tank, after sedimentation qualified adjacent ammonia
Yl benzoic acid methyl esters, this methyl o-aminobenzoate mass content should be greater than 98%;
3, doazo reaction: add methyl esters and the add mass ratio of water be 1:2 water, unlatching simultaneously in doazo reaction still
Interlayer salt solution starts cooling, then add methyl esters with add hydrochloric acid mass ratio be the hydrochloric acid that 1:2.7 and mass concentration are 30%;
In methyl esters mixing kettle, add methyl esters and the add mass ratio of the water water that is 1:1.5, open interlayer steam heating simultaneously, open stirring add mass content be greater than 99% left and right and methyl esters and add the Sodium Nitrite that the mass ratio of Sodium Nitrite is 1:0.5, molten
Separate, then the mass content of step 2 gained is greater than to 98% methyl o-aminobenzoate and adds in methyl esters mixing kettle, stir, observe emulsification situation, generate methyl esters Sodium Nitrite mixed solution, the temperature of this mixed solution should be controlled between 20～24 ℃;
Open lumping weight nitrogen reactor interlayer salt water for cooling, when hydrochloric acid soln temperature is down to below 25 ℃, start to add the methyl esters Sodium Nitrite mixed solution of above-mentioned gained.Carry out doazo reaction, in reaction process, temperature should be controlled at below 30 ℃, after this reaction finishes, obtains the light yellow diazo liquid of clear, with starch, refers to that K1 indicator test should show blue.
4, replacement(metathesis)reaction: the diazo liquid of step 3 > gained is squeezed in replacement reaction kettle, open stirring, open replacement(metathesis)reaction interlayer salt water for cooling, add mass content be greater than 94% and methyl esters and add copper sulfate mass ratio be the copper sulfate of 1:0.2 proportional quantity, when temperature is down to 20 ℃, pass into methyl esters with the mass ratio of the logical sulfurous gas proportional quantity sulfurous gas that is 1:0.8.In logical sulfurous gas process, replacement reaction kettle still pressure should be at 0-0.1MPa, temperature should be at 30-50 ℃, the logical sulfurous gas time should be carried out replacement(metathesis)reaction at 70-90 minute, after logical sulfurous gas finishes, close and stir, close salt solution, in temperature, be 45 ℃ of left and right, pressure is to be incubated 90 minutes under the condition about 0.1 MPa, obtains adjacent-sulfinic acid methyl benzoate, with the adjacent-sulfinic acid methyl benzoate of H acid reagent test, should not develop the color;
5, chlorination reaction: be the industrial toluene of 1:2 proportional quantity toward adding the mass ratio of methyl esters and institute's processing industry toluene in above-mentioned replacement reaction kettle, open stirring, open salt water for cooling.When temperature is down to 20-30 ℃, start to pass into methyl esters with the mass ratio of logical liquid chlorine be the liquid chlorine of 1:0.3 proportional quantity.In logical liquid chlorine process, temperature should be at 40-50 ℃, after logical liquid chlorine finishes, with the adjacent SULPHURYL CHLORIDE methyl benzoate of p-diaminodiphenyl ethanol reagent test, orange be should show, stirring, salt solution closed, standing, after layering, sour water is emitted, obtain adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution, be pressed in aminating reaction still;
6, aminating reaction: be incorporated as adjacent sulphonyl chlorobenzene first in the adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution obtaining to chlorination reaction
The toluene that acid methyl esters toluene solution is 0.6 times, stirs, and sedimentation, divides lower floor's sour water only, opens stirring, uses salt water for cooling.When temperature is down to 10-20 ℃, in aminating reaction still, pass into liquefied ammonia, carry out aminating reaction, in logical liquefied ammonia process, temperature must not be higher than 95 ℃, during question response liquid bleach, stop logical liquefied ammonia, survey pH value 7-8 o'clock, aminating reaction reaches terminal, obtains adjacent sulfonamide benzoic acid methyl esters;
7, washing, drying: stop stirring, standing, extract upper toluene out aminating reaction still, then add the adjacent sulfonamide benzoic acid methyl esters of water washing, treat NH in washing water
4 +< 2.5/ ten thousand o'clock, dries, and must dry adjacent sulfonamide benzoic acid methyl esters;
8, neutralization reaction: the water that the mass ratio that adds water and adjacent sulfonamide benzoic acid methyl esters in neutralization reaction still is 1:1, open stirring, add the adjacent sulfonamide benzoic acid methyl esters of the drying obtaining after drying, in temperature, must not surpass under the condition of 85 ℃, slowly add sodium hydroxide solution, measured reaction liquid pH value was at 6.5-7.5 o'clock, stop hydro-oxidation sodium solution, neutralization reaction reaches terminal, soluble saccharin solution degree Beaume during temperature 60 C is 25-40Be, through decolouring, filter, concentrated, crystallization, drying, the dry finished product soluble saccharin that to obtain.
The present invention adopts aforementioned production method, it take phthalic anhydride as raw material through amidation, esterification, diazotization, displacement, chlorination, ammonification, neutralization, decolouring, concentrated, crystallization, drying, after dry soluble saccharin finished product, and aminating reaction is wherein to take the adjacent SULPHURYL CHLORIDE methyl benzoate that liquefied ammonia obtains with chlorination reaction as raw material to react the adjacent sulphonyl aminobenzoic acid methyl esters of generation.This production method can shorten production process route, reduces production link, reduces production costs, and can also reduce the ammonia nitrogen quantity discharged in factory effluent, and every production 1moL soluble saccharin can reduce 1moLNH
4 +discharge, makes ammonia nitrogen quantity discharged in factory effluent can reduce 50%, is conducive to environment protection.
Accompanying drawing explanation
Accompanying drawing is a kind of process flow sheet of production method of soluble saccharin.
Embodiment
Below in conjunction with accompanying drawing, describe the specific embodiment of the present invention in detail.
According to process flow sheet, the concrete technology step of production method of the present invention is as follows:
1, amidate action: putting into phthalic anhydride in amidate action still is the ammoniacal liquor of 1:0.1 proportional quantity with the mass ratio that institute adds ammoniacal liquor, the condensation salt water for cooling of opening stirring, air draft, being-15 ℃ of left and right by temperature.When temperature is down to 0 ℃ of left and right, open phthalic anhydride hopper baffle plate, about 10 minutes, add phthalic anhydride, add phthalic anhydride amount and ammoniacal liquor mass ratio be 1:0.1.When temperature rises to 50-70 ℃, pH value is 7 o'clock, and slowly adding mass concentration is the liquid caustic soda solution of 30% left and right, when pH value is 9, stops hydro-oxidation sodium solution, and reaction outlet temperature is 85 ℃ of left and right.Close cooling salt solution, insulation 20-50 minute.After insulation finishes, ammonia excretion obtains qualified amidation liquid about 1 hour, and amidation liquid free alkali mass concentration is 0.08-0.25%.
2, esterification: the qualified amidation liquid of gained is squeezed in reaction kettle of the esterification, opened stirring, open salt water for cooling, this brine temp is-15 ℃ of left and right.When temperature is down to 30 ℃, add phthalic anhydride with add methyl alcohol mass ratio be the methyl alcohol of 1:1.5 proportional quantity, methyl alcohol density is 0.791-0.793g/cm
3.When temperature is down to below 10 ℃, add phthalic anhydride with add clorox mass ratio be the chlorine bleach liquor of 1:5 proportional quantity, chlorine bleach liquor's mass concentration is 14% left and right.Add in chlorine bleach liquor's process, temperature of reaction must not surpass 30 ℃, in reaction process, with KI reagent examination look, if colour-fast, illustrates that reaction has reached terminal, stops adding chlorine bleach liquor.Close salt solution, when temperature rises to 40 ℃ of left and right, the hot water that adds appropriate approximately 100 ℃, close and stir, standing about 20 minutes, after layering, upper strata methyl o-aminobenzoate is squeezed in methyl esters slurry tank, sedimentation obtains qualified methyl o-aminobenzoate after 48 hours, methyl o-aminobenzoate mass content should be greater than 98%.
3, doazo reaction: adding methyl esters and the mass ratio that institute adds water in doazo reaction still is the water of 1:2 proportional quantity, opens interlayer salt solution and starts cooling, then adding mass concentration is 30% hydrochloric acid, methyl esters and add hydrochloric acid mass ratio be 1:2.7.
In methyl esters hybrid reactor, add methyl esters with add water mass ratio be the water of 1:1.5 proportional quantity, open interlayer steam heating simultaneously, open stir add mass content be greater than 99% left and right and methyl esters and add Sodium Nitrite mass ratio be the Sodium Nitrite of 1:0.5 proportional quantity, after dissolving, mass content being greater than to 98% methyl o-aminobenzoate adds in methyl esters mixing kettle, stir sampling after 10-20 minutes and observe emulsification degree, emulsification degree should maintain 1 minute not stratified being advisable, obtain methyl esters Sodium Nitrite mixed solution, the temperature of this mixed solution should be controlled between 20～24 ℃.
Open lumping weight nitrogen reactor interlayer salt water for cooling, when hydrochloric acid soln temperature is down to below 25 ℃, start to add above-mentioned gained methyl esters Sodium Nitrite mixed solution.A temperature of every 10 minutes records, temperature should be controlled at below 30 ℃.After doazo reaction finishes, sampling should show blue with the test of KI Starch Indicator, illustrates that doazo reaction reaches terminal, obtains the light yellow diazo liquid of clear.
4, replacement(metathesis)reaction: the light yellow diazo liquid of above-mentioned gained clear is squeezed in replacement reaction kettle, open stirring, open interlayer salt water for cooling, add mass content be greater than 94% and methyl esters and add copper sulfate mass ratio be the copper sulfate of 1:0.2 proportional quantity, when temperature is down to 20 ℃, pass into methyl esters with the mass ratio of logical sulfurous gas be the sulfurous gas of 1:0.8 proportional quantity.In logical sulfurous gas process, reactor still pressure should be at 0-0.1MPa, and temperature should be at 30-50 ℃, and the logical sulfurous gas time should be at 70-90 minute.After logical sulfurous gas finishes, close stirring, salt solution.At pressure, be 0.1 MPa left and right, temperature is under the condition of 45 ℃ of left and right, should be incubated 90 minutes, after insulation finishes, obtains adjacent-sulfinic acid methyl benzoate.With the adjacent-sulfinic acid methyl benzoate of H acid reagent test, should not develop the color.
5, chlorination reaction: toward add in above-mentioned replacement reaction kettle methyl esters with add toluene mass ratio be the industrial toluene of 1:2 proportional quantity, open stirring, open salt water for cooling.When temperature is down to 20-30 ℃, start to pass into methyl esters with the mass ratio of logical liquid chlorine be the liquid chlorine of 1:0.3 proportional quantity.In logical liquid chlorine process, temperature should be at 40-50 ℃, and the time is about 90 minutes, after logical liquid chlorine finishes, with the adjacent SULPHURYL CHLORIDE methyl benzoate of p-diaminodiphenyl ethanol reagent test, should show orange.Close stirring, salt solution, standing about 30 minutes, after layering, sour water is emitted, adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution is pressed in aminating reaction still.
6, aminating reaction: add toluene to being equipped with in the aminating reaction still of adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution, add toluene amount be 0.6 times of adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution, stir 10-30 minutes, sedimentation 3-6 hours, divides the lower floor's sour water in the anti-empty still of ammonification only.
Open stirring, open salt water for cooling.When temperature is down to 10-20 ℃, under temperature must not be higher than the condition of 95 ℃, in aminating reaction still, pass into liquefied ammonia, during question response liquid bleach, stop logical liquefied ammonia, surveying pH value is 7-8 o'clock, aminating reaction reaches terminal, obtains adjacent sulfonamide benzoic acid methyl esters.
7, washing, drying: stop stirring, standing 30-, after 50 minutes, extracts upper toluene out aminating reaction still, then add the adjacent sulfonamide benzoic acid methyl esters of water washing, treats NH in washing water
4 +< 2.5/ ten thousand o'clock, dries, and must dry adjacent sulfonamide benzoic acid methyl esters.
8, neutralization reaction: the mass ratio that adds water and adjacent sulfonamide benzoic acid methyl esters in neutralization reaction still is the water of 1:1 proportional quantity, open stirring, add the adjacent sulfonamide benzoic acid methyl esters obtaining after drying, in temperature, must not surpass under the condition of 85 ℃, slowly add sodium hydroxide solution, measured reaction liquid pH value, when 6.5-7.5, stops hydro-oxidation sodium solution, reaction reaches terminal, obtains soluble saccharin solution.Degree Beaume during 60 ℃ of soluble saccharin solution is 25-40Be.By this soluble saccharin solution according to a conventional method through decolouring, filter, concentrated, crystallization, drying, dry etc. finished product soluble saccharin.
Claims (1)
1. a production method for soluble saccharin, is characterized in that following processing step:
1 >, amidate action: by mass concentration be about 16% ammoniacal liquor and water by phthalic anhydride with add ammoniacal liquor mass ratio be 1:0.1 proportional quantity is put into amidate action still, open stirring, air draft, condensation salt water for cooling, when temperature is down to 0 ℃ of left and right, the phthalic anhydride of the proportional quantity that to add by the mass ratio of phthalic anhydride and ammoniacal liquor be 1:0.1, add phthalic anhydride, when temperature rises to 50-70 ℃, during pH value 7, slowly adding mass concentration is the sodium hydroxide solution of 30% left and right, when pH value is 9, stop hydro-oxidation sodium solution, in the outlet temperature of amidate action during 85 ℃ of left and right, close cooling salt solution, insulation, ammonia excretion, obtain qualified amidation liquid,
2 >, esterification: above-mentioned amidation liquid is squeezed in reaction kettle of the esterification, open stirring, open salt water for cooling, when temperature is down to 30 ℃, add phthalic anhydride with add methyl alcohol mass ratio be the methyl alcohol of 1:1.5 proportional quantity, when temperature is down to below 10 ℃, add phthalic anhydride with add clorox mass ratio be that 1:5 and mass concentration are the chlorine bleach liquor of 14% proportional quantity, add in chlorine bleach liquor's process, temperature of reaction must not be over 30 ℃, in reaction process, with K1 reagent, try look, colour-fast, esterification reaches terminal, stop adding chlorine bleach liquor, close salt solution, when temperature rises to 40 ℃ of left and right, the hot water that adds appropriate approximately 100 ℃, close and stir, standing, after layering, upper strata methyl o-aminobenzoate is squeezed in methyl esters slurry tank, after sedimentation, separate mother liquor and obtain qualified methyl o-aminobenzoate, this methyl o-aminobenzoate mass content should be greater than 98%,
3 >, doazo reaction: in doazo reaction still, add methyl esters and the add mass ratio of the water water that is 1:2, open interlayer salt solution and start cooling, then add methyl esters with add hydrochloric acid mass ratio be that 1:2.7 and mass concentration are the hydrochloric acid of 30% proportional quantity
In methyl esters mixing kettle, add methyl esters and the add mass ratio of the water water that is 1:1.5, open interlayer steam heating simultaneously, open stirring, add mass content be greater than 99% left and right and methyl esters and add Sodium Nitrite mass ratio be the Sodium Nitrite of 1:0.5 proportional quantity, dissolve, then the mass content of step 2 > gained is greater than to 98% methyl o-aminobenzoate and adds in methyl esters mixing kettle, stir, observe emulsification degree, in mixing process, temperature should be controlled between 20～24 ℃;
Open lumping weight nitrogen reactor salt water for cooling, when hydrochloric acid soln temperature is down to below 25 ℃, start to add methyl esters and the Sodium Nitrite mixed solution of above-mentioned gained, temperature should be controlled at below 30 ℃, carry out doazo reaction, after this reaction finishes, obtain the light yellow diazo liquid of clear, with starch KI indicator test, should show blue
4 >, replacement(metathesis)reaction: the diazo liquid of step 3 > gained is squeezed in replacement reaction kettle, open stirring, open replacement reaction kettle interlayer salt water for cooling, add mass content be greater than 94% and methyl esters and add copper sulfate mass ratio be the copper sulfate of 1:0.2 proportional quantity, when temperature is down to 20 ℃, pass into methyl esters with the mass ratio of logical sulfurous gas be the sulfurous gas of 1:0.8 proportional quantity, in logical sulfurous gas process, replacement reaction kettle pressure should be at 0-0.1MPa, temperature should be at 30-50 ℃, the logical sulfurous gas time should be at 70-90 minute, carry out replacement(metathesis)reaction, after logical sulfurous gas finishes, close and stir, close salt solution, in temperature, be 45 ℃ of left and right, pressure is to be incubated 90 minutes under the condition about 0.1 MPa, obtain adjacent-sulfinic acid methyl benzoate, with the adjacent-sulfinic acid methyl benzoate of H acid reagent test, should not develop the color,
5 >, chlorination reaction: be the industrial toluene of 1:2 proportional quantity toward adding the mass ratio of methyl esters and institute's processing industry toluene in above-mentioned replacement reaction kettle, open stirring, open salt water for cooling, when temperature is down to 20-30 ℃, start to pass into methyl esters with the mass ratio of logical liquid chlorine be the liquid chlorine of 1:0.3 proportional quantity, in logical liquid chlorine process, temperature should be at 40-50 ℃, after logical liquid chlorine finishes, with the adjacent SULPHURYL CHLORIDE methyl benzoate of p-diaminodiphenyl ethanol reagent test, should show orange, close and stir, salt solution, standing, after layering, sour water is emitted, obtain adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution, be pressed in aminating reaction still,
6 >, aminating reaction: the industrial toluene that is incorporated as 0.6 times of adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution in the adjacent SULPHURYL CHLORIDE methyl benzoate toluene solution obtaining to chlorination reaction, stir, sedimentation, lower floor's sour water is divided only, open stirring, use salt water for cooling, when temperature is down to 10-20 ℃, in aminating reaction still, pass into liquefied ammonia, carry out aminating reaction, in logical liquefied ammonia process, temperature must not be higher than 95 ℃, during question response liquid bleach, stop logical liquefied ammonia, survey pH value 7-8 o'clock, aminating reaction reaches terminal, obtains adjacent sulfonamide benzoic acid methyl esters;
7 >, washing, drying: stop stirring, standing, extract upper toluene out aminating reaction still, then add the adjacent sulfonamide benzoic acid methyl esters of water washing, treat NH in washing water
4 +< 2.5/ ten thousand o'clock, dries, and must dry adjacent sulfonamide benzoic acid methyl esters;
8 >, neutralization reaction: the water that the mass ratio that adds water and adjacent sulfonamide benzoic acid methyl esters in neutralization reaction still is 1: 1, open stirring, add the adjacent sulfonamide benzoic acid methyl esters of the drying obtaining after drying, in temperature, must not surpass under the condition of 85 ℃, slowly add sodium hydroxide solution, measured reaction liquid pH value is when 6.5-7.5, stop hydro-oxidation sodium solution, neutralization reaction reaches terminal, during temperature 60 C soluble saccharin solution degree Beaume be 25-40Be, through decolouring, filter, concentrated, crystallization, drying, the dry finished product soluble saccharin that to obtain.
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