CN103044489B - A kind of synthetic method of 3-nitro-4-phenol-arsonic acid - Google Patents
A kind of synthetic method of 3-nitro-4-phenol-arsonic acid Download PDFInfo
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Abstract
The invention discloses a kind of synthetic method of 3-nitro-4-phenol-arsonic acid: comprise condensation reaction, reclaim dewatering agent, obtain the steps such as condensated liquid, cooled and filtered, recycling, hydrolysis, acidifying, filtration, adjustment PH, crystallisation by cooling, centrifuge dehydration, oven dry, 3-nitro-4-phenol-arsonic acid synthetic method of the present invention is simple to operate, raw material availability is high, low cost, reclaim mother liquor can reuse, environmental friendliness.
Description
Technical field
The invention belongs to chemical field, specifically a kind of synthetic method of 3-nitro-4-phenol-arsonic acid.
Background technology
Roxarsone (chemical name: 3-nitro-4-phenol-arsonic acid), be light yellow, odorless, tasteless crystalline powder, belong to organic arsenic class fodder additives, be mainly used in chicken, in the feed of pig, as additive for farm animal feed, it not only plays the trophicity effect of supplementary essential trace element arsenic, it also has important drug effect, the synthesis of protein can be promoted, change the metabolism of intestinal cell, suppress the growth of unwanted bacteria in enteron aisle, play the effect such as growth stimulant and antiseptic-germicide, it is a kind of multifunctional feed additive of high safety, in the U.S., Canada, Latin America, many countries and regions such as South East Asia are widely applied.According to the report of the authoritative magazine Feed Stuffs of feed circle, at usage quantity comparatively many three times of the microbiotic of U.S.'s roxarsone, be most economical organic arsenic.
China is an Animal husbandry production big country, and roxarsone has obtained the common recognition of vast cultivation producer as economic, efficient, multi-functional fodder additives.The roxarsone that Zhejiang Rongyao Chemical Industry Co., Ltd produces, due to of fine qualities, has become domestic brand product.The roxarsone that our company produces makes an addition in broiler chicken feed through herding institute of the Chinese Academy of Agricultural Sciences, carries out simultaneous test and shows to significantly improve feed conversion rate, and simultaneously also to show to add arsenic preparation in chicken feed the most remarkable with roxarsone for test-results.
Roxarsone, because of its significant effect, brings huge economic benefit to feedstuff industry.The complete feed of China in 2005 reaches 6,000 ten thousand tons according to statistics, and add if press 30---50PPM, need roxarsone 1800-3000 ton every year, this product has very large market potential at home as seen.This product also can export to many countries and regions such as the U.S., Canada, Latin America, South East Asia simultaneously, earns foreign exchange save foreign exchange for country.
The consumption of original 3-nitro-4-phenol-arsonic acid synthesis technique Raw is large, utilization ratio is low, and reaction solution cannot be recycled, and wastewater treatment trouble
Summary of the invention
The present invention seeks to large for the consumption of original 3-nitro-4-phenol-arsonic acid synthesis technique Raw, utilization ratio is low, reaction solution cannot be recycled, and the problems such as wastewater treatment trouble, provides a kind of 3-nitro-4-phenol-arsonic acid synthetic method.
The technical solution used in the present invention is:
A kind of synthetic method of 3-nitro-4-phenol-arsonic acid, comprise the steps: that o-Nitraniline mixes with arsenic acid, at dewatering agent A, under 135 ~ 160 DEG C of conditions, normal pressure condensation reaction is carried out under the effect of auxiliary agent A, after reacting completely, normal pressure reclaims dewatering agent, obtain condensated liquid, add water in condensated liquid and dilute, stir 0.5 ~ 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, described filter cake A and 3-nitro-Ponazuril, described filtrate A recycles, described filter cake A adds water and is warming up to 70 DEG C and adds alkali lye and regulate pH value 4-14, after adsorbent, less than 55 DEG C filtrations are chilled to after dissolving, obtain filter cake B and liquor B, described liquor B adds alkali and is hydrolyzed, obtained 3-nitro-4-phenol-arsonic acid sodium, add acid and carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, described liquor C is filtered after adsorbent, centrifuge dehydration after filtrate crystallisation by cooling, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, is characterized in that the mass ratio that feeds intake of described o-Nitraniline and dewatering agent A and auxiliary agent A is 1:0. 1 ~ 0.16:0.005 ~ 0.008.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that described o-Nitraniline and the arsenic acid mass ratio that feeds intake is 1:5 ~ 12, preferred 1:9 ~ 11, described arsenic acid mixes with o-Nitraniline A with the form of 85% arsenate solution.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, is characterized in that the mass ratio that feeds intake of described condensated liquid and water is 1:3.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that described dewatering agent A is polyacrylamide, zellon, 4a molecular sieve or trichloromethane, described auxiliary agent A is cycloheptaamylose, hydrazine hydrate, n-caprylic acid, palmitinic acid or lauric acid.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that the method that described filtrate A recycles is: filtrate A filters after adsorbent, filtrate is concentrated into temperature to 136 DEG C, obtain and reclaim mother liquor, described recovery mother liquor is as raw material for the preparation of 3-nitro-Ponazuril, and in described recovery mother liquor, the mass concentration of arsenic acid is 75 ~ 85%.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that described alkali is the oxyhydroxide of metal or oxide compound, the oxyhydroxide of alkaline-earth metal or oxide compound and the aqueous solution thereof, belonging to alkali be preferably sodium carbonate or sodium hydroxide or its solution, described acid is hydrochloric acid, sulfuric acid or nitric acid.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that described sorbent material is take carbonaceous as various acticarbon and metal, the nonmetal oxide class sorbent material of raw material; Described sorbent material is preferably silica gel, activated alumina, gac, molecular sieve.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that described recovery mother liquor for the preparation of the method for 3-nitro-4-phenol-arsonic acid is: mother liquor will be reclaimed, arsenic acid and o-Nitraniline, dewatering agent B and auxiliary agent B mixing, be heated with stirring to 145 ~ 150 DEG C, condensation reaction is carried out under condition of normal pressure, after condensation reaction terminates, reclaim dewatering agent, obtain condensated liquid, add water in condensated liquid and dilute, stir 0.5 ~ 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, described filter cake A and 3-nitro-Ponazuril, described filtrate A recycles, described filter cake A adds water and is warming up to 70 DEG C and adds alkali lye and regulate pH value 4-14, after adsorbent, less than 55 DEG C filtrations are chilled to after dissolving, obtain filter cake B and liquor B, described liquor B adds alkali and is hydrolyzed, obtained 3-nitro-4-phenol-arsonic acid sodium, add acid and carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, described liquor C is filtered after adsorbent, centrifuge dehydration after filtrate crystallisation by cooling, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid.
The synthetic method of described 3-nitro-4-phenol-arsonic acid, it is characterized in that described o-Nitraniline B and dewatering agent B and the auxiliary agent B mass ratio that feeds intake is 1:0. 1 ~ 0.16:0.005 ~ 0.008, arsenic acid adds with the form of mass concentration 85% arsenate solution, o-Nitraniline is 1:5.60 ~ 6.0 with reclaiming arsenic acid mass ratio in mother liquor, described dewatering agent B is polyacrylamide or trichloromethane, described auxiliary agent B is cycloheptaamylose, and described recovery mother liquor can reuse.
Crystallisation by cooling method of the present invention is technology well known in the art, usually adopts and utilizes thermal junction crystallization to carry out recrystallization.
The inventive method is simple to operate, and raw material availability is high, low cost, and reclaiming mother liquor can reuse, environmental friendliness, pollutes few.
Accompanying drawing explanation
Fig. 1 is the liquid chromatogram of product 3-nitro-4-phenol-arsonic acid of the present invention.
Embodiment
Embodiment 1:
500kg arsenate solution (mass concentration 85%) is added in 2000L enamel kiln, 100kg o-Nitraniline, 10kg trichloromethane, 0.5kg cycloheptaamylose, after ready, open to stir and heat up, temperature of reaction controls at 135 ~ 160 DEG C, start to react timing, about 5.5 hours reaction times, after reaction terminates, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 0.5h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 4 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding sulfuric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5, crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 110kg.
Embodiment 2:
1200kg arsenate solution (mass concentration 85%) is added in 2000L enamel kiln, 100kg o-Nitraniline, 10kg polyacrylamide, 0.5kg cycloheptaamylose, after ready, open to stir and heat up, temperature of reaction controls at 135 ~ 160 DEG C, start to react timing, about 5.0 hours reaction times, after reaction terminates, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 0.5h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 12 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding hydrochloric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 115kg.
Embodiment 3:
900kg arsenate solution (mass concentration 85%) is added in 2000L enamel kiln, 100kg o-Nitraniline, 10kg zellon, 0.5kg n-caprylic acid, after ready, open to stir and heat up, temperature of reaction controls at 135 ~ 160 DEG C, start to react timing, about 5.5 hours reaction times, after reaction terminates, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 14 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding sulfuric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 112kg.
Embodiment 4:
750kg arsenate solution (mass concentration 85%) is added in 2000L enamel kiln, 100kg o-Nitraniline, 10kg4a molecular sieve, 0.5kg hydrazine hydrate, after ready, open to stir and heat up, temperature of reaction controls at 135 ~ 160 DEG C, start to react timing, about 5.0 hours reaction times, after reaction terminates, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 11 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding hydrochloric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 108kg.
Embodiment 5:
The recovery mother liquor obtained in embodiment 3 is first dropped in 2000L enamel kiln, mend punching again and add 100kg arsenic acid, o-Nitraniline 100kg and 16kg polyacrylamide, 0.8kg n-caprylic acid is heated to 135 ~ 160 DEG C under whipped state, react 5 hours, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 6 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding hydrochloric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 120kg.
Embodiment 6:
The recovery mother liquor obtained in embodiment 2 is first dropped in 2000L enamel kiln, mend punching again and add 150kg arsenic acid, o-Nitraniline 100kg and 16kg trichloromethane, 0.8kg cycloheptaamylose is heated to 135 ~ 160 DEG C under whipped state, react 5.5 hours, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 9 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding sulfuric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 125kg.
Embodiment 7:
The recovery mother liquor obtained in embodiment 5 is first dropped in 2000L enamel kiln, mend punching again and add 100kg arsenic acid, o-Nitraniline 100kg and 16kg zellon, 0.8kg palmitinic acid is heated to 135 ~ 160 DEG C under whipped state, react 5.0 hours, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 0.5h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 6 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding hydrochloric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 114kg.
Embodiment 8:
The recovery mother liquor obtained in embodiment 7 is first dropped in 2000L enamel kiln, mend punching again and add 150kg arsenic acid, o-Nitraniline 100kg and 16kg polyacrylamide, 0.8kg cycloheptaamylose is heated to 135 ~ 160 DEG C under whipped state, react 5.5 hours, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 12 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding hydrochloric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 128kg.
Embodiment 9:
The recovery mother liquor obtained in embodiment 8 is first dropped in 2000L enamel kiln, mend punching again and add 150kg arsenic acid, o-Nitraniline 100kg and 16kg4a molecular sieve, 0.8kg cycloheptaamylose is heated to 135 ~ 160 DEG C under whipped state, react 5.0 hours, close steam, normal pressure concentration and recovery dewatering agent, obtain concentrated solution, add water in condensated liquid and carry out analysing releasing, stir 0.5h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, filter cake A is 3-nitro-Ponazuril condensation material, filtrate A recycles, filter cake A add water be warming up to 70 DEG C add liquid caustic soda regulate pH value 7 dissolve after after adsorbent, be chilled to 55 DEG C of filtrations, obtain filter cake B and liquor B filtrate, B filtrate adds alkali and is hydrolyzed, regular hour and thermotonus, obtained 3-nitro-4-phenol-arsonic acid sodium, adding sulfuric acid regulates pH value about 4.8 to carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, liquor C is filtered after adsorbent, filtrate regulates PH about 2.5 crystallisation by cooling, centrifuge dehydration, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid 118kg.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., be all included within protection scope of the present invention.
Claims (8)
1. the synthetic method of a 3-nitro-4-phenol-arsonic acid, it is characterized in that comprising the steps: that o-Nitraniline mixes with arsenic acid, at dewatering agent A, under 135 ~ 160 DEG C of conditions, normal pressure condensation reaction is carried out under the effect of auxiliary agent A, after reacting completely, normal pressure reclaims dewatering agent, obtain condensated liquid, add water in condensated liquid and dilute, stir 0.5 ~ 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, described filter cake A and 3-nitro-Ponazuril, described filtrate A recycles, described filter cake A adds water and is warming up to 70 DEG C and adds alkali lye adjust ph 4-14, after adsorbent, less than 55 DEG C filtrations are chilled to after dissolving, obtain filter cake B and liquor B, described liquor B adds alkali and is hydrolyzed, obtained 3-nitro-4-phenol-arsonic acid sodium, add acid and carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, described liquor C is filtered after adsorbent, centrifuge dehydration after filtrate crystallisation by cooling, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid, described dewatering agent A is polyacrylamide, zellon, 4a molecular sieve or trichloromethane, described auxiliary agent A is cycloheptaamylose, hydrazine hydrate, n-caprylic acid, palmitinic acid or lauric acid.
2. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 1, is characterized in that the mass ratio that feeds intake of described o-Nitraniline and dewatering agent A and auxiliary agent A is 1:0. 1 ~ 0.16:0.005 ~ 0.008.
3. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 1, it is characterized in that described o-Nitraniline and the arsenic acid mass ratio that feeds intake is 1:5 ~ 12, described arsenic acid mixes with o-Nitraniline A with the form of 85% arsenate solution.
4. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 1, is characterized in that the mass ratio that feeds intake of described condensated liquid and water is 1:3.
5. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 1, it is characterized in that the method that described filtrate A recycles is: filtrate A filters after adsorbent, filtrate is concentrated into temperature to 136 DEG C, obtain and reclaim mother liquor, described recovery mother liquor is as raw material for the preparation of 3-nitro-Ponazuril, and in described recovery mother liquor, the mass concentration of arsenic acid is 75 ~ 85%.
6. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 1, it is characterized in that described filter cake A add water be warming up to 70 DEG C add alkali lye adjust ph 4-14 and described liquor B add alkali be hydrolyzed in alkali be the oxyhydroxide of metal or oxide compound and the aqueous solution thereof, described 3-nitro-4-phenol-arsonic acid sodium, adding the acid acid carried out in acidifying is hydrochloric acid, sulfuric acid or nitric acid.
7. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 1, is characterized in that described sorbent material is silica gel, activated alumina, gac or molecular sieve.
8. the synthetic method of 3-nitro-4-phenol-arsonic acid as claimed in claim 5, it is characterized in that described recovery mother liquor for the preparation of the method for 3-nitro-4-phenol-arsonic acid is: mother liquor will be reclaimed, arsenic acid and o-Nitraniline B, dewatering agent B and auxiliary agent B mixing, be heated with stirring to 145 ~ 150 DEG C, condensation reaction is carried out under condition of normal pressure, after condensation reaction terminates, reclaim dewatering agent, obtain condensated liquid, add water in condensated liquid and dilute, stir 0.5 ~ 1h, obtain reaction solution, reaction solution cooled and filtered, obtain filter cake A and filtrate A, described filter cake A and 3-nitro-Ponazuril, described filtrate A recycles, described filter cake A adds water and is warming up to 70 DEG C and adds alkali lye adjust ph 4-14, after adsorbent, less than 55 DEG C filtrations are chilled to after dissolving, obtain filter cake B and liquor B, described liquor B adds alkali and is hydrolyzed, obtained 3-nitro-4-phenol-arsonic acid sodium, add acid and carry out acidifying, after reaction terminates, filter, obtain filter cake C and liquor C, described liquor C is filtered after adsorbent, centrifuge dehydration after filtrate crystallisation by cooling, precipitation is dried, obtain 3-nitro-4-phenol-arsonic acid, described o-Nitraniline B and dewatering agent B and the auxiliary agent B mass ratio that feeds intake is 1:0. 1 ~ 0.16:0.005 ~ 0.008, arsenic acid adds with the form of mass concentration 85% arsenate solution, o-Nitraniline is 1:5.60 ~ 6.0 with reclaiming arsenic acid mass ratio in mother liquor, described dewatering agent B is polyacrylamide or trichloromethane, described auxiliary agent B is cycloheptaamylose, described recovery mother liquor can reuse.
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