CN113020094B - Method and device for automatic washing of violuric acid - Google Patents
Method and device for automatic washing of violuric acid Download PDFInfo
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- CN113020094B CN113020094B CN202110223914.4A CN202110223914A CN113020094B CN 113020094 B CN113020094 B CN 113020094B CN 202110223914 A CN202110223914 A CN 202110223914A CN 113020094 B CN113020094 B CN 113020094B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/14—Removing waste, e.g. labels, from cleaning liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
- C07D239/60—Three or more oxygen or sulfur atoms
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- Organic Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
本发明提供了一种紫脲酸自动洗涤的方法，根据紫脲酸含量或紫脲酸溶料后的滤液pH对物料进行分类洗涤；本发明还提供了一种实现紫脲酸自动洗涤的装置；本发明解决了传统水洗紫脲酸仅可去除紫脲酸中水溶性杂质的难题，减轻了紫脲酸所带杂质对后续加氢还原的影响；实现了紫脲酸的分类、分等级清洗，减少有机溶剂及洗涤水用量。
The invention provides a method for automatic washing of murexuric acid, wherein materials are washed in a classified manner according to the content of murexuric acid or the pH value of a filtrate after the murexuric acid is dissolved in the material; the invention also provides a device for realizing automatic washing of murexuric acid; the invention solves the problem that conventional water washing of murexuric acid can only remove water-soluble impurities in murexuric acid, and reduces the influence of impurities carried by murexuric acid on subsequent hydrogenation reduction; the classification and graded washing of murexuric acid is realized, and the consumption of organic solvent and washing water is reduced.
Description
Technical Field
The invention belongs to the field of chemical pharmacy, and particularly relates to a method and a device for automatically washing purple urea acid.
Background
The caffeine synthesis process using cyanoacetic acid and dimethylurea as the starting materials has the advantages of simple process, high yield, good intermediate stability and the like, and becomes the main stream production process of caffeine series products. The purple urea acid is produced by ring closure and nitrosation of dimethylurea and cyanoacetic acid, is an important intermediate for producing caffeine series products, and the content and impurity level of the purple urea acid directly influence the subsequent hydrogenation reduction reaction, thereby influencing the yield and quality of the caffeine series products. How to reduce the impurity level in the reaction system before the hydrogenation reduction becomes a serious issue in improving the yield of the quality of the caffeine product.
At present, in order to reduce the influence of the purple urea acid on a nickel catalyst in a hydrogenation reduction system, water-soluble impurities in the purple urea acid are mainly washed by adopting a clear water washing mode, but organic impurities in the purple urea acid cannot be effectively removed, and researches prove that part of organic impurities in the purple urea acid can be hydrolyzed under alkaline conditions, hydrolysis products are condensed with a subsequent intermediate dimethyl-FAU to form a ring, and under the catalysis of residual nickel in the presence of light and oxygen, the hydrolysis is carried out to generate a carboxylic acid compound under the presence of subsequent alkali and acid, so that the quality of caffeine finished products is seriously influenced.
The patent (CN 101812024B) discloses a purification method of dimethylvioluric acid, specifically, alcohol, ether or ketone organic solvents are mixed with water and soluble zinc salts are added to realize the washing of the violuric acid, the content of the violuric acid can be increased to more than 90 percent from 60 percent, but the disclosed method stays in a laboratory research stage, and organic solvents such as methanol, tertiary butanol, acetone and the like used in the disclosed method can remain in caffeine, thereby causing the exceeding of organic impurities in caffeine finished products, and the introduction of halogen elements such as zinc chloride, zinc bromide and the like can also influence an impurity system, so that the method obviously has a large risk for caffeine with dual properties of medicines and foods. The washed purple urea acid still has 10 percent of impurities, and the residual impurities still affect the subsequent hydrogenation reduction reaction.
Disclosure of Invention
The invention provides an automatic washing method of purple urea acid, which comprises the steps of classifying and washing materials according to the content of the purple urea acid or the pH value of filtrate after the dissolution of the purple urea acid:
(1) Washing by a first method when the content of the purple urea acid is >95% (w/w) or when the pH of a filtrate obtained by dispersing the purple urea acid in purified water is > 4;
(2) And when the content of the purple urea acid is less than or equal to 95% (w/w) and the pH value of the filtrate obtained by dispersing the purple urea acid in the purified water is less than or equal to 4, washing by adopting a second method.
The first method comprises the following washing steps:
(1) Dispersing the purple urea acid and water in a solvent tank V1 according to the mass ratio of 1:3, stirring for 10-15 minutes until the materials are dispersed uniformly, pressing the materials into a washing tank V2-1 by using compressed air, stirring for 10 minutes, opening the washing tank V2-1, compressing air, and extruding 2/3 washing water;
(2) After the pressure is finished, adding water to the original volume in a washing tank V2-1, stirring for 10 minutes, then opening compressed air, and extruding 2/3 washing water to a filtrate collecting tank V4-1;
(3) After the pressure is finished, adding water to the original volume in a washing tank V2-1, stirring for 10 minutes, then opening compressed air, and extruding 2/3 washing water to a filtrate washing tank V4-1;
(4) And monitoring the pH value of the washing water for the third time, if the pH value is more than 6.5, finishing washing, adding water into the material in the washing tank V2-1 to supplement the original volume, and transferring the material to the pulping tank V3-1 for pulping for later use.
The second method comprises the following washing steps:
(1) Dispersing the purple urea acid and water in a solution tank V1 according to the mass ratio of 1:2, stirring for 10-15 minutes until the materials are dispersed uniformly, pressing the materials to a washing tank V2-2 by using compressed air, stirring for 10 minutes, opening the washing tank V2-2 to compress the air, and extruding 1/2 washing water to a filtrate collecting tank V4-1;
(2) Adding the solvent in the auxiliary solvent tank V5-1 and the saline solution in the auxiliary solvent tank V5-2 into the washing tank V2-2, supplementing the volume of the raw material, stirring for 15 minutes, then opening compressed air, and extruding 3/4 washing liquid into the filtrate collecting tank V4-2;
(3) After the pressing is finished, adding water to 1.5 times of the volume of the raw material in a washing tank V2-2, stirring for 10 minutes, then opening compressed air, and extruding 2/3 washing water to a filtrate washing tank V4-2;
(4) After the pressing is finished, adding water to 1.5 times of the volume of the raw material in a washing tank V2-2, stirring for 10 minutes, then opening compressed air, and extruding 2/3 washing water to a filtrate washing tank V4-1;
(5) And monitoring the pH value of the washing water for the fifth time, if the pH value is more than 6.5, finishing washing, adding water into the material in the washing tank V2-2 to make up to 1.5 times of the volume of the raw material, and transferring the material to the pulping tank V3-2 for pulping for later use.
The invention also provides a device for realizing automatic washing of the purple urea acid, which comprises 1 dissolving tank V1, 2 washing tanks V2-1 and V2-2, 2 beating tanks V3-1 and V3-2, 2 filtrate collecting tanks V4-1 and V4-2,2 auxiliary solvent tanks V5-1 and V5-2, wherein the dissolving tank V1 is connected with the washing tank V2-1 and the washing tank V2-2, the washing tank V2-1 is connected with the beating tank V3-1, the washing tank V2-1 is connected with the filtrate collecting tank V4-1, the washing tank V2-2 is connected with the beating tank V3-2, the beating tank V3-2 is connected with the filtrate collecting tanks V4-1 and V4-2, and the auxiliary solvent tanks V5-1 and V5-2 are respectively connected with the washing tank V2-2.
All tank bodies of the automatic purple urea acid washing device are provided with liquid level meters, a dissolving tank, a washing tank and a pulping tank are respectively provided with double-layer stirring, wherein the washing tank is provided with a pressure meter, a connecting pipeline of the washing tank and a filtrate collecting tank is provided with a pH monitoring meter, and the pH monitoring meter, the pressure meter and the liquid level count value can be automatically controlled through PLC.
The solvent in the auxiliary solvent tank V5-1 is ethanol with the volume fraction of more than 99 percent;
And the auxiliary solvent tank V5-2 is internally provided with a saturated aqueous solution of salt solution zinc sulfate.
The method solves the problem that the traditional water-washing purple urea acid only can remove water-soluble impurities in the purple urea acid, lightens the influence of the impurities carried by the purple urea acid on subsequent hydrogenation reduction, realizes classification and hierarchical cleaning of the purple urea acid, reduces the consumption of an organic solvent and washing water, and also determines salts and the organic solvent suitable for the washing of the purple urea acid.
Drawings
FIG. 1 is a schematic diagram of an automatic washing process flow of the purple urea acid, wherein V1 is a dissolution tank, V2-1 and V2-2 are washing tanks, V3-1 and V3-2 are beating tanks, V4-1 and V4-2 are filtrate collecting tanks, V5-1 and V5-2 are auxiliary solvent tanks, liquid level meters (L1, L2-2, L3-1, L3-2, L4-1, L4-2), double-layer stirring (M1, M2-2, M3-1, M3-2), pH monitors (pH-1, pH-2), and pressure meters (P2-1 and P2-2).
Detailed Description
The following further description, taken in conjunction with the accompanying drawings, is not intended to limit the scope of the invention, and specific embodiments thereof are as follows:
Example 1:
According to detection, the absolute content of the purple urea acid is 96.21%, a first washing method is adopted for washing, 500kg of purple urea acid is put into a solution tank V1, 1500L of water dispersion solution is added, after stirring for 13 minutes, the material is pressed into a washing tank V2-1 by compressed air for washing, after stirring for 10 minutes, the washing tank V2-1 is opened for compressed air, 1000L of water is pressed out, after adding 1000L of water into the washing tank V2-1, after stirring for 10 minutes, the compressed air is opened, 1000L of washing water is pressed out to a filtrate collecting tank V4-1, after adding 1000L of water into the washing tank V2-1 again, after stirring for 10 minutes, the compressed air is opened, 1000L of washing water is pressed out to a filtrate collecting tank V4-1, after detecting the pH value of the washing water for the third time is 6.75, after washing, 1000L of water is added into the washing tank V2-1, and the material is transferred into a beating tank V3-1 for standby. And (3) carrying out suction filtration and drying on the purple urea acid in the pulping tank V3-1, and then carrying out absolute content detection, wherein the detection result is 99.85%, and the yield is 97.82% when the washed purple urea acid is used for hydrogenation reduction reaction.
Example 2:
According to detection, the absolute content of the purple urea acid is 94.85%, 100g of the purple urea acid is dispersed in 300mL of water, the pH value of the filtrate is measured to be 4.23, a first washing method is adopted for washing, 500kg of the purple urea acid is put into a solution tank V1, 1500L of water dispersion solvent is added, after stirring for 12 minutes, the material is pressed into a washing tank V2-1 by compressed air for washing, after stirring for 10 minutes, the washing tank V2-1 is opened for compressed air, 1000L of water is pressed out, 1000L of water is added into the washing tank V2-1, after stirring for 10 minutes, 1000L of washing water is pressed out into a filtrate collecting tank V4-1, after stirring for 10 minutes, 1000L of washing water is pressed out into the filtrate collecting tank V4-1, the pH value of the third washing water is detected to be 6.83, after stirring, 1000L of water is added into the washing tank V2-1, and the material is transferred into a beating tank V3-1 for standby. And (3) carrying out suction filtration and drying on the purple urea acid in the pulping tank V3-1, and then carrying out absolute content detection, wherein the detection result is 99.65%, and the yield is 96.92% when the washed purple urea acid is used for hydrogenation reduction reaction.
Example 3:
Detecting that the absolute content of the purple urea acid is 93.68%, dispersing 100g of the purple urea acid in 300mL of water, measuring the pH of the filtrate to be 4.02, washing by adopting a second washing method, adding 500kg of the purple urea acid into a solution tank V1, adding 1000L of water dispersion solvent, stirring for 15 minutes, pressing the material into a washing tank V2-2 by using compressed air for washing, stirring for 10 minutes, opening the washing tank V2-2 for compressed air, pressing 500L of washing water into a filtrate collecting tank V4-1, adding the solvent 300L in an auxiliary solvent tank V5-1 and the saline solution 200L in the auxiliary solvent tank V5-2 into the washing tank V2-2, stirring for 15 minutes, opening the compressed air, pressing 750L of washing liquid into a filtrate collecting tank V4-2, adding 1250L of water into the washing tank V2-2, stirring for 10 minutes, opening the compressed air, pressing 1000L of washing water into the filtrate washing tank V4-2, adding 1000L of water into the washing tank V2-2, stirring for 10 minutes, pressing 500L of washing water into the filtrate collecting tank V4-1, pressing the filtrate into the washing tank V2, detecting the pH of the filtrate after stirring for 1000L of the washing tank V2-2, and beating the filtrate, detecting the pH after the washing tank is finished, and the washing water is equal to 3L to 3-6. And (3) carrying out suction filtration and drying on the purple urea acid in the pulping tank V3-2, and then carrying out absolute content detection, wherein the detection result is 99.72%, and the yield is 97.03% when the washed purple urea acid is used for hydrogenation reduction reaction.
Claims (3)
1. A method for automatically washing the purple urea acid is characterized in that the material is washed in a classified manner according to the content of the purple urea acid or the pH value of filtrate after the purple urea acid is dissolved:
(1) When the mass percentage content of the purple urea acid is more than 95 percent or the pH value of the filtrate obtained by dispersing the purple urea acid in the purified water is more than 4, the first method is adopted for washing;
(2) When the mass percentage of the purple urea acid is less than or equal to 95 percent and the pH value of the filtrate obtained by dispersing the purple urea acid in the purified water is less than or equal to 4, washing by adopting a second method;
the first method comprises the following washing steps:
1) Dispersing the purple urea acid and water in a solution tank (V1) according to the mass ratio of 1:3, stirring for 10-15 minutes until the materials are dispersed uniformly, pressing the materials to a first washing tank (V2-1) by using compressed air, stirring for 10 minutes, and opening the first washing tank (V2-1) to compress air to extrude 2/3 washing water;
2) After the pressure is finished, adding water to the original volume in a first washing tank (V2-1), stirring for 10 minutes, then opening compressed air, and extruding 2/3 washing water to a first filtrate collecting tank (V4-1);
3) After the pressure is finished, adding water to the original volume in a first washing tank (V2-1), stirring for 10 minutes, then opening compressed air, and extruding 2/3 washing water to a first filtrate collecting tank (V4-1);
4) Monitoring the pH value of the washing water for the third time, if the pH value is more than 6.5, finishing washing, adding water into the material of the first washing tank (V2-1) to supplement the original volume, and transferring the material to the first pulping tank (V3-1) for pulping for later use;
the second method comprises the following washing steps:
① Dispersing the purple urea acid and water in a solution tank (V1) according to the mass ratio of 1:2, stirring for 10-15 minutes until the materials are dispersed uniformly, pressing the materials to a second washing tank (V2-2) by using compressed air, stirring for 10 minutes, opening the second washing tank (V2-2) to compress air, and extruding 1/2 washing water to a first filtrate collecting tank (V4-1);
② Adding the solvent in the first auxiliary solvent tank (V5-1) and the saline solution in the second auxiliary solvent tank (V5-2) into the second washing tank (V2-2), supplementing the volume of the original solvent, stirring for 15 minutes, then opening compressed air, and extruding 3/4 washing liquid to the second filtrate collecting tank (V4-2);
③ After the pressing is finished, adding water into the second washing tank (V2-2) to 1.5 times of the volume of the original solution, stirring for 10 minutes, then opening compressed air, and pressing out 2/3 of washing water to the second filtrate collecting tank (V4-2);
④ After the pressing is finished, adding water to 1.5 times of the volume of the raw solution in a second washing tank (V2-2), stirring for 10 minutes, then opening compressed air, and pressing out 2/3 washing water to a first filtrate collecting tank (V4-1);
⑤ Monitoring the pH value of the washing water for the fifth time, if the pH value is more than 6.5, finishing washing, adding water into the material in the second washing tank (V2-2) to be supplemented to 1.5 times of the volume of the raw material, and transferring the material to the second pulping tank (V3-2) for pulping for later use;
the automatic washing device comprises 1 dissolving tank (V1), a first washing tank (V2-1), a second washing tank (V2-2), a first pulping tank (V3-1), a second pulping tank (V3-2), a first filtrate collecting tank (V4-1), a second filtrate collecting tank (V4-2), a first auxiliary solvent tank (V5-1) and a second auxiliary solvent tank (V5-2), wherein the dissolving tank (V1) is connected with the first washing tank (V2-1) and the second washing tank (V2-2), the first washing tank (V2-1) is connected with the first pulping tank (V3-1), the first washing tank (V2-1) is connected with the first filtrate collecting tank (V4-1), the second washing tank (V2-2) is connected with the second pulping tank (V3-2), the second pulping tank (V3-2) is connected with the first filtrate collecting tank (V4-1) and the second filtrate collecting tank (V4-2), and the first auxiliary solvent tank (V2-2) is connected with the second filtrate collecting tank (V2-2).
2. The method for automatic washing of purple urea acid according to claim 1, wherein: all tank bodies are provided with liquid level meters, a solution tank (V1), a first washing tank (V2-1), a second washing tank (V2-2), a first pulping tank (V3-1), a second pulping tank (V3-2) are respectively provided with a first double-layer stirring (M1), a second double-layer stirring (M2-1), a third double-layer stirring (M2-2), a fourth double-layer stirring (M3-1) and a fifth double-layer stirring (M3-2), wherein the first washing tank (V2-1) and the second washing tank (V2-2) are provided with a first pressure meter (P2-1) and a second pressure meter (P2-2), and the first washing tank (V2-1), the second washing tank (V2-2) and a first filtrate collecting tank (V4-1) and a second filtrate collecting tank (V4-2) are connected with a connecting pipe line, and the first pH monitor (pH-1), the second pH monitor (pH-2), the first pH monitor (pH-1), the second pH monitor (P-2), the second pH monitor (P2) and the first pH monitor (P-1), the second pH monitor (P-2) are provided with a first pressure meter (P2-1) and a second pressure meter (P2-2), and a second pressure meter (P-2), and a first pressure meter (P-2) and a second pressure meter (P-2), and a second pressure meter (P-tank and a second filtrate tank.
3. The method for automatically washing the purple urea acid according to claim 1, wherein the solvent in the first auxiliary solvent tank (V5-1) is ethanol with the volume fraction of more than 99%, and the salt solution in the second auxiliary solvent tank (V5-2) is a saturated aqueous solution of zinc sulfate.
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| GB1446603A (en) * | 1972-09-22 | 1976-08-18 | Kayaba Industry Co Ltd | Method for the recycle treatment of waste water from chromium plating |
| CA2240030A1 (en) * | 1997-06-10 | 1998-12-10 | Praxair Technology, Inc. | Method for washing bleached wood pulp |
| JP3378228B2 (en) * | 2000-06-30 | 2003-02-17 | 住友重機械工業株式会社 | Countercurrent multistage washing method for pulp |
| CN101380633B (en) * | 2008-10-10 | 2010-06-02 | 北京化工大学 | A washing and separating device for washing water jacket and its application |
| CN105085231A (en) * | 2014-05-20 | 2015-11-25 | 天华化工机械及自动化研究设计院有限公司 | Treatment method of acetic acid solvent in oxidation unit of PTA industrial equipment |
| CN104550099B (en) * | 2014-12-18 | 2016-07-06 | 广州飞机维修工程有限公司 | Aircarrier aircraft kitchen water boiling device automatic cleaning system |
| CN107602310B (en) * | 2017-10-30 | 2020-05-29 | 西安近代化学研究所 | Air whistle type continuous flooding acid washing method suitable for explosives |
| CN109761208B (en) * | 2019-03-06 | 2020-07-07 | 深圳海纳百川科技有限公司 | Iron phosphate washing process and device |
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