CN105585192B - A kind of method of wastewater treatment of 4,6 dihydroxy-pyrimidine production - Google Patents
A kind of method of wastewater treatment of 4,6 dihydroxy-pyrimidine production Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C07—ORGANIC CHEMISTRY
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- 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
- C07D239/52—Two oxygen atoms
- C07D239/54—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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Abstract
The invention discloses a kind of method of wastewater treatment of 4,6 dihydroxy-pyrimidines production, it is related to 4,6 dihydroxy-pyrimidine production technical fields.This method is that processing produces waste water caused by 4,6 dihydroxy-pyrimidines using formic acid acidization, and adding excessive formic acid into 4,6 dihydroxy-pyrimidine sodium salt solutions under stirring is acidified, and separation of solid and liquid obtains 4,6 dihydroxy-pyrimidine products and waste water；Industrial caustic soda is added into waste water under stirring, neutralization reaction occurs, neutralizes excessive formic acid, pH value is adjusted to 6~9；Waste water after neutralization is subjected to rectifying and steams alcohol, obtains by-product industrial methanol；It will be separated except the waste water after alcohol, obtain byproduct sodium formate.Provided by the invention a kind of 4, the method for wastewater treatment of 6 dihydroxy-pyrimidines production, qualified 4,6 dihydroxy-pyrimidine products can not only be obtained, moreover it is possible to which sodium formate and methanol effectively in recovery waste water, production and cost recovery are low, simple to operate, non-secondary pollution.
Description
Technical field
The present invention relates to 4,6- dihydroxy-pyrimidine production technical fields.
Background technology
4,6- dihydroxy-pyrimidines are fine chemical materials, medicine intermediate, as organic synthesis intermediate, in medical industry
In be used for produce sulfonamides sulfamonomethoxine, and the intermediate of adenine phosphate, antineoplastic and adjuvant class.Main production
Process is to obtain product 4 with hydrochloric acid acidifying pyrimidine sodium salt, 6- dihydroxy-pyrimidines, often produces one ton of 4,6- dihydroxy-pyrimidine finished product,
10 tons or so of waste water, wherein formic acid sodium content 10% will be produced, the waste water belongs to high salt organic waste water, can not carry out biochemistry
Processing, the usual way of manufacturing enterprise is by Waste water concentrating, obtains the salt-mixture of sodium chloride and sodium formate, although this method completes
Effective processing of waste water, utility therein can not but be recycled, such as sodium formate therein, at present world market demand
At 800,000 tons or so, it is mainly used in the industry such as sodium hydrosulfite, oxalic acid, formic acid, papermaking, food, medicine, abroad the first of significant proportion
Sour sodium is used as Snow Agent and antifreezing agent.
The content of the invention
The technical problem to be solved in the present invention is to be directed to above-mentioned the deficiencies in the prior art, there is provided one kind 4,6- dihydroxy-pyrimidines
The method of wastewater treatment of production, qualified 4,6- dihydroxy-pyrimidine products can not only be obtained, moreover it is possible to the first effectively in recovery waste water
Sour sodium and methanol, production and cost recovery are low, simple to operate, non-secondary pollution, suitable for the extensive of 4,6- dihydroxy-pyrimidines
The waste water treatment of production.
In order to solve the above technical problems, the technical solution used in the present invention is：A kind of 4,6- dihydroxy-pyrimidines production
Method of wastewater treatment is processing using waste water, the production of formic acid acidization caused by formic acid acidization production 4,6- dihydroxy-pyrimidines
Refer to, adding excessive formic acid into 4,6- dihydroxy-pyrimidine sodium salt solutions under stirring is acidified, and main reaction formula is
C4H2N2O2Na2 + 2HCOOH→C4H4N2O2+ 2HCOONa, separation of solid and liquid is carried out after reaction, obtain the production of 4,6- dihydroxy-pyrimidines
Product and 4,6- dihydroxy-pyrimidine waste water；Industrial caustic soda is added into 4,6- dihydroxy-pyrimidine waste water under stirring, in generation
And reaction, excessive formic acid is neutralized, the pH value of 4,6- dihydroxy-pyrimidine waste water is adjusted to 6~9；Waste water after neutralization is carried out
Alcohol is steamed in rectifying, obtains by-product industrial methanol and except 4, the 6- dihydroxy-pyrimidine waste water after alcohol；By except the 4,6- dihydroxy after alcohol it is phonetic
Pyridine waste water separates, and obtains byproduct sodium formate.
Preferably, the remaining mother liquor after isolated byproduct sodium formate is returned into set to except 4, the 6- dihydroxy-pyrimidines after alcohol give up
In water.
Preferably, except 4, the 6- dihydroxy-pyrimidine waste water after alcohol is separated into, by except 4, the 6- dihydroxy-pyrimidine waste water after alcohol
It is concentrated under reduced pressure, carries out separation of solid and liquid, obtain byproduct sodium formate.
Preferably, the water steamed during being concentrated under reduced pressure returns set into 4,6- dihydroxy-pyrimidine sodium salt solutions.
Preferably, industrial caustic soda is sodium hydroxide or sodium carbonate, the main reaction formula of neutralization reaction for HCOOH+NaOH →
HCOONa + H2O or 2HCOOH+Na2CO3 →2HCOONa + H2O + CO2。
Preferably, it is 7~8.5 to neutralize pH value.
It is using beneficial effect caused by above-mentioned technical proposal：A kind of 4,6- dihydroxy-pyrimidines life provided by the invention
The method of wastewater treatment of production, qualified 4,6- dihydroxy-pyrimidine products can not only be obtained, moreover it is possible to it is phonetic effectively to reclaim 4,6- dihydroxy
Sodium formate and methanol in pyridine waste water, and simple to operate, non-secondary pollution, raw materials for production use formic acid, make the reaction in waste water
Product is more single, while 4,6- dihydroxy-pyrimidine product qualities are ensured, effectively reduces production and cost recovery, reclaims formic acid
The product quality of sodium can reach industrial standard, and method of the invention can be suitably used for the large-scale production of 4,6- dihydroxy-pyrimidines
Waste water treatment.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.
The method of wastewater treatment of 4,6- of one kind dihydroxy-pyrimidines production is processing using formic acid acidization production 4,6- dihydroxies
Waste water caused by yl pyrimidines, the production of formic acid acidization refer to, and it is phonetic to be continuously added to 4,6- dihydroxy into reactor under stirring
Pyridine sodium salt solution and 85% excessive by-product formic acid, carry out acidification reaction, main reaction formula is C4H2N2O2Na2 + 2HCOOH→
C4H4N2O2+ 2HCOONa, separation of solid and liquid is carried out after reaction, obtain 4,6- dihydroxy-pyrimidines product and 4,6- dihydroxy-pyrimidine give up
Water, the main component in the waste water is sodium formate, methanol and a small amount of organic impurities.
Embodiment 1
（1）Sodium hydroxide is added into 4,6- dihydroxy-pyrimidine waste water under stirring, neutralization reaction occurs, neutralized
The formic acid of amount, neutralization reaction formula are HCOOH+NaOH → HCOONa+H2O, adjust the pH value of 4,6- dihydroxy-pyrimidine waste water
Save as 7；
（2）To step（1）Waste water after neutralization carries out rectifying and steams alcohol, obtains by-product industrial methanol, methanol content is
98%, residue removes 4, the 6- dihydroxy-pyrimidine waste water after alcohol；
（3）By step（2）In remove 4, the 6- dihydroxy-pyrimidine waste water after alcohol and be concentrated under reduced pressure, then carry out separation of solid and liquid,
Byproduct sodium formate is obtained, formic acid sodium content is 97%, and remaining wastewater mother liquor is returned into set to step（2）In remove alcohol after 4,6- bis-
In hydroxy pyrimidine waste water, the water steamed during being concentrated under reduced pressure returns set into 4,6- dihydroxy-pyrimidine sodium salt solutions.
Embodiment 2
（1）Sodium hydroxide is added into 4,6- dihydroxy-pyrimidine waste water under stirring, neutralization reaction occurs, neutralized
The formic acid of amount, neutralization reaction formula are HCOOH+NaOH → HCOONa+H2O, adjust the pH value of 4,6- dihydroxy-pyrimidine waste water
Save as 8；
（2）To step（1）Waste water after neutralization carries out rectifying and steams alcohol, obtains by-product industrial methanol, methanol content is
95%, residue removes 4, the 6- dihydroxy-pyrimidine waste water after alcohol；
（3）By step（2）In remove 4, the 6- dihydroxy-pyrimidine waste water after alcohol and be concentrated under reduced pressure, then carry out separation of solid and liquid,
Byproduct sodium formate is obtained, formic acid sodium content is 95%, and remaining wastewater mother liquor is returned into set to step（2）In remove alcohol after 4,6- bis-
In hydroxy pyrimidine waste water, the water steamed during being concentrated under reduced pressure returns set into 4,6- dihydroxy-pyrimidine sodium salt solutions.
Embodiment 3
（1）Sodium hydroxide is added into 4,6- dihydroxy-pyrimidine waste water under stirring, neutralization reaction occurs, neutralized
The formic acid of amount, neutralization reaction formula are HCOOH+NaOH → HCOONa+H2O, adjust the pH value of 4,6- dihydroxy-pyrimidine waste water
Save as 9；
（2）To step（1）Waste water after neutralization carries out rectifying and steams alcohol, obtains by-product industrial methanol, methanol content is
93%, residue removes 4, the 6- dihydroxy-pyrimidine waste water after alcohol；
（3）By step（2）In remove 4, the 6- dihydroxy-pyrimidine waste water after alcohol and be concentrated under reduced pressure, then carry out separation of solid and liquid,
Byproduct sodium formate is obtained, formic acid sodium content is 93.6%, and remaining wastewater mother liquor is returned into set to step（2）In remove alcohol after 4,6-
In dihydroxy-pyrimidine waste water, the water steamed during being concentrated under reduced pressure returns set into 4,6- dihydroxy-pyrimidine sodium salt solutions.
Embodiment 4
（1）Sodium hydroxide is added into 4,6- dihydroxy-pyrimidine waste water under stirring, neutralization reaction occurs, neutralized
The formic acid of amount, neutralization reaction formula are 2HCOOH+Na2CO3 →2HCOONa + H2O + CO2, 4,6- dihydroxy-pyrimidines is given up
The pH value of water is adjusted to 6；
（2）To step（1）Waste water after neutralization carries out rectifying and steams alcohol, obtains by-product industrial methanol, methanol content is
90%, residue removes 4, the 6- dihydroxy-pyrimidine waste water after alcohol；
（3）By step（2）In remove 4, the 6- dihydroxy-pyrimidine waste water after alcohol and be concentrated under reduced pressure, then carry out separation of solid and liquid,
Byproduct sodium formate is obtained, formic acid sodium content is 93%, and remaining wastewater mother liquor is returned into set to step（2）In remove alcohol after 4,6- bis-
In hydroxy pyrimidine waste water, the water steamed during being concentrated under reduced pressure returns set into 4,6- dihydroxy-pyrimidine sodium salt solutions.
Embodiment 5
（1）Sodium hydroxide is added into 4,6- dihydroxy-pyrimidine waste water under stirring, neutralization reaction occurs, neutralized
The formic acid of amount, neutralization reaction formula are 2HCOOH+Na2CO3 →2HCOONa + H2O + CO2, 4,6- dihydroxy-pyrimidines is given up
The pH value of water is adjusted to 8.5；
（2）To step（1）Waste water after neutralization carries out rectifying and steams alcohol, obtains by-product industrial methanol, methanol content is
92%, residue removes 4, the 6- dihydroxy-pyrimidine waste water after alcohol；
（3）By step（2）In remove 4, the 6- dihydroxy-pyrimidine waste water after alcohol and be concentrated under reduced pressure, then carry out separation of solid and liquid,
Byproduct sodium formate is obtained, formic acid sodium content is 93%, and remaining wastewater mother liquor is returned into set to step（2）In remove alcohol after 4,6- bis-
In hydroxy pyrimidine waste water, the water steamed during being concentrated under reduced pressure returns set into 4,6- dihydroxy-pyrimidine sodium salt solutions.
The method of wastewater treatment for 4, the 6- dihydroxy-pyrimidines production that embodiments of the invention provide, can be suitably used for 4,6- dihydroxies
The waste water treatment of the large-scale production of yl pyrimidines, it can not only efficiently produce qualified 4,6- dihydroxy-pyrimidine products, moreover it is possible to effectively
The sodium formate and methanol in 4,6- dihydroxy-pyrimidine waste water, simple to operate, non-secondary pollution are reclaimed, raw materials for production use by-product first
Acid, production cost is effectively reduced, and make the reaction product in waste water more single, recovery is convenient and cost is low, reclaims sodium formate
Product quality can reach industrial standard.
Above technical characteristic constitutes highly preferred embodiment of the present invention, and there is stronger adaptability and optimal implementation to imitate for it
Fruit, can be according to the non-essential technical characteristic of increase and decrease be actually needed, to meet the needs of different situations.
Claims (5)
1. one kind 4, the method for wastewater treatment of 6- dihydroxy-pyrimidines production, it is characterised in that：It is that processing is given birth to using formic acid acidization
Waste water caused by 4,6- dihydroxy-pyrimidines is produced, the formic acid acidization production refers to, to 4,6- dihydroxy-pyrimidines under stirring
Add excessive formic acid in sodium salt solution to be acidified, main reaction formula is C4H2N2O2Na2+2HCOOH→C4H4N2O2+ 2HCOONa,
Separation of solid and liquid is carried out after reaction, obtains 4,6- dihydroxy-pyrimidines product and 4,6- dihydroxy-pyrimidine waste water；Under stirring to
Industrial caustic soda is added in 4, the 6- dihydroxy-pyrimidines waste water, neutralization reaction occurs, neutralizes excessive formic acid, makes 4, the 6- bis-
The pH value of hydroxy pyrimidine waste water is adjusted to 6~9；Waste water after neutralization is subjected to rectifying and steams alcohol, by-product industrial methanol is obtained and removes
4,6- dihydroxy-pyrimidine waste water after alcohol；After 4, the 6- dihydroxy-pyrimidine waste water except after alcohol is concentrated under reduced pressure, carry out
Separation of solid and liquid, obtain byproduct sodium formate.
2. the method for wastewater treatment of a kind of 4,6- dihydroxy-pyrimidines production according to claim 1, it is characterised in that will divide
Set is returned into the 4,6- dihydroxy-pyrimidine waste water removed after alcohol from the remaining mother liquor after the byproduct sodium formate is obtained.
3. the method for wastewater treatment of a kind of 4,6- dihydroxy-pyrimidines production according to claim 1, it is characterised in that described
The water steamed during being concentrated under reduced pressure returns set into the 4,6- dihydroxy-pyrimidines sodium salt solution.
4. the method for wastewater treatment of a kind of 4,6- dihydroxy-pyrimidines production according to claim 1, it is characterised in that described
Industrial caustic soda is sodium hydroxide or sodium carbonate, and the main reaction formula of the neutralization reaction is HCOOH+NaOH → HCOONa+H2O or
2HCOOH+Na2CO3→2HCOONa+H2O+CO2。
5. the method for wastewater treatment of a kind of 4,6- dihydroxy-pyrimidines production according to claim 1, it is characterised in that described
It is 7~8.5 to neutralize pH value.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1214044A (en) * | 1996-05-17 | 1999-04-14 | 曾尼卡有限公司 | Process for making 4,6-dihydroxypyrimidine |
| CN101081715A (en) * | 2007-04-06 | 2007-12-05 | 广东中成化工股份有限公司 | Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process |
| CN101696192A (en) * | 2009-10-15 | 2010-04-21 | 沈阳化工学院 | Pyrimidine substituted acrylic ester compounds with fungicidal activities and preparation method thereof |
| CN102115463A (en) * | 2010-01-05 | 2011-07-06 | 重庆紫光化工股份有限公司 | Method for synthesizing 4,6-dihydroxy pyrimidine |
| CN103641077A (en) * | 2013-12-16 | 2014-03-19 | 浙江嘉成化工有限公司 | Recycling method of sodium hydrosulfite wastewater |
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- 2015-12-25 CN CN201510985196.9A patent/CN105585192B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1214044A (en) * | 1996-05-17 | 1999-04-14 | 曾尼卡有限公司 | Process for making 4,6-dihydroxypyrimidine |
| CN101081715A (en) * | 2007-04-06 | 2007-12-05 | 广东中成化工股份有限公司 | Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process |
| CN101696192A (en) * | 2009-10-15 | 2010-04-21 | 沈阳化工学院 | Pyrimidine substituted acrylic ester compounds with fungicidal activities and preparation method thereof |
| CN102115463A (en) * | 2010-01-05 | 2011-07-06 | 重庆紫光化工股份有限公司 | Method for synthesizing 4,6-dihydroxy pyrimidine |
| CN103641077A (en) * | 2013-12-16 | 2014-03-19 | 浙江嘉成化工有限公司 | Recycling method of sodium hydrosulfite wastewater |
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