CN1179413A - Method for producing formic acid and coproducing various sodium phosphate salts by acidifying sodium formate with perphosphoric acid - Google Patents
Method for producing formic acid and coproducing various sodium phosphate salts by acidifying sodium formate with perphosphoric acid Download PDFInfo
- Publication number
- CN1179413A CN1179413A CN 97103209 CN97103209A CN1179413A CN 1179413 A CN1179413 A CN 1179413A CN 97103209 CN97103209 CN 97103209 CN 97103209 A CN97103209 A CN 97103209A CN 1179413 A CN1179413 A CN 1179413A
- Authority
- CN
- China
- Prior art keywords
- acid
- formic acid
- sodium
- sodium phosphate
- phosphate salts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 title claims abstract description 80
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 235000019253 formic acid Nutrition 0.000 title claims abstract description 40
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 title claims abstract description 22
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 title claims abstract description 16
- 239000004280 Sodium formate Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 235000019254 sodium formate Nutrition 0.000 title claims abstract description 14
- 239000002253 acid Substances 0.000 title claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims abstract 2
- 230000005494 condensation Effects 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- MPNNOLHYOHFJKL-UHFFFAOYSA-N peroxyphosphoric acid Chemical compound OOP(O)(O)=O MPNNOLHYOHFJKL-UHFFFAOYSA-N 0.000 claims description 9
- 239000006227 byproduct Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- NFIYTPYOYDDLGO-UHFFFAOYSA-N phosphoric acid;sodium Chemical compound [Na].OP(O)(O)=O NFIYTPYOYDDLGO-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 2
- 230000000996 additive effect Effects 0.000 claims 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical compound Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- -1 compound phosphoric acid sodium salts Chemical class 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000005649 metathesis reaction Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000011734 sodium Substances 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract 3
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 abstract 1
- 229920000137 polyphosphoric acid Polymers 0.000 abstract 1
- 229940005657 pyrophosphoric acid Drugs 0.000 abstract 1
- 229910000162 sodium phosphate Inorganic materials 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 235000019832 sodium triphosphate Nutrition 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 1
- 229910000318 alkali metal phosphate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940045641 monobasic sodium phosphate Drugs 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
A new process method for producing formic acid and coproducing various sodium phosphate salts by using sodium formate acidified by superphosphoric acid. Mixing a certain amount of perphosphoric acid and a certain amount of sodium formate, performing double decomposition reaction by using the high chemical energy of the first hydrogen ion in the acid to generate formic acid, evaporating out the formic acid, and recovering the finished product by condensation, wherein Na is+Ions with H in phosphoric acid2PO－ 4Ions, pyrophosphoric acid (radical) ions and polyphosphoric acid (radical) ions to form NaH2PO4The compound sodium phosphate salt can be used for preparing various sodium phosphate salts through simple treatment. The production cost is low (the cost of 1.325 tons of soda ash is saved when one ton of formic acid is produced), the operation of the new technological process is convenient, and the equipment is similar to and simple as the traditional process.
Description
The invention belongs to the manufacture method of aliphatic carboxylic acid and alkali metal phosphate.
In making the prior art of formic acid, remove oxo process " methyl-formiate " method, the yellow phosphoric tail gas that domestic most employing is traditional or contain all kinds of coal gas and the white liquor synthesising acid sodium of CO is again with vitriol oil acidifying production formic acid.The main drawback of these class methods is: the formic acid concn that (1) produces is generally 85%; By product industry saltcake added value is low, and consumes valuable these basic chemical raw materials of the vitriol oil, thereby benefit is also low.(2) careless manipulation in the acidization, vitriol oil part too much easily cause formic acid to decompose.
In addition, domestic in recent years " formic acid and oxalic acid communication " (first phase in June, 1991) have article " formic acid coproduction five sodium test pre-tests " and " Shaanxi chemical industry " (1991 the 5th phases) to have the article experimental study of formic acid " the phosphoric acid method synthetic " and " phosphate industry " (1994 the 4th phases) that article documents such as " commerical tests of formic acid coproduction phosphoric acid salt novel process " is arranged.The former thinking intangibility; The not mentioned phosphoric acid concentration of the latter; The phosphoric acid that middle person proposes with 85% and 94% replaces the vitriol oil; Referring to simultaneously with the omnidistance rewinding of 85% phosphoric acid acidifying sodium formate is 70% aqueous formic acid of lower concentration, the strong phosphoric acid acidifying sodium formate with 94% " omnidistance rewinding is the finished product formic acid more than 85% ".70% aqueous formic acid also needs three road successive extracting rectifyings, and very trouble is also uneconomical.Even so-called 94% the phosphoric acid acidifying sodium formate " omnidistance rewinding is the product formic acid more than 85% " that uses, its theoretical value reaches 86% only, and this also can't guarantee suitability for industrialized production.Moreover the amount that formic acid that acidifying sodium formate adds is done end acid do not introduced in article.Learn that by practice the strong phosphoric acid acidifying sodium formate with 94% not only returns formic acid or formic acid is made end acid amount greatly, and it is very difficult with batch mixing industrialization operation to feed intake, (in other words, be not that to be fixed up be exactly the formic acid that constantly returns into a large amount of), the production cycle is very long, and blowing is also very difficult.
The objective of the invention is to overcome the deficiency of above-mentioned technology, adopt peroxophosphoric acid (total P
2O
5By 69.6%～86.9%) as the breakthrough means of acidifying sodium formate.Its reaction process is following carries out:
(1) at first drops into a certain amount of peroxophosphoric acid, under agitation add the part of sodium formiate expense; Controlled temperature is no more than 45 ℃, also can be higher, but should below the formic acid boiling temperature, carry out.
(2) return throwing formic acid, concentration 85%～90% all can; Returning acid gets final product on a small quantity.Under agitation continue to add remaining sodium formiate.
(3) stir, improve temperature of reaction kettle fast, blowing is in the formic acid distillation still rapidly.
(4) in still kettle, steam formic acid, by being condensed into product, while evaporate to dryness by product NaH
2PO
4--compound phosphoric acid sodium, by product discharging.
(5) by product is made into 40% aqueous solution of being permitted in about 80 ℃, and the heavy fast foreign material that remove are put into Flavouring jar, adjust P
2O
5Content as the feed liquid of producing Sodium hexametaphosphate 99.
(6) by product is adjusted pH value with the waste lye and the phosphoric acid of soda ash or synthesising acid sodium, and heat treated is adjusted sodium salt.Get final product production SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, tertiary sodium phosphate, trisodium phosphate, tripoly phosphate sodium STPP and various compound phosphoric acid sodium salt.
Method of the present invention compared with prior art has following advantage: 1 compares with vitriol oil acidifying sodium formate:
Production cost is low.One ton of formic acid of every production is equivalent to save the expense (one ton of formic acid of every production needs one ton of 100% caustic soda, and one ton of caustic soda is equivalent to 1.325 tons of soda ash) of 1.325 tons of soda ash.2 compare with 94% phosphoric acid acidifying sodium formate: 2.1 acidizations are easy, smooth, it is few to return the acid amount, can realize industrialization; 2.2 the formic acid concn height, omnidistance rewinding can reach more than the 89%-96%; 3 these methods can be produced and meet GB first grade Sodium hexametaphosphate 99.
Description of drawings:
Accompanying drawing 1 is produced formic acid by-product NaH for the peroxophosphoric acid acidifying sodium formate
2PO
4--compound phosphoric acid sodium salt process flow diagram:
Accompanying drawing 2 is the NaH with by-product
2PO
4--the compound phosphoric acid sodium salt is made various sodium phosphate salt process flow diagrams.
Claims (6)
1 one kinds are utilized peroxophosphoric acid (total P
2O
5By 69.6%～86.9%) acidifying sodium formate production formic acid, the method for the various sodium phosphate salts of coproduction.It is characterized in that: peroxophosphoric acid reacts with the sodium formiate mixing earlier, utilizes first hydrionic chemical energy metathesis sodium formiate in the acid, makes it to be converted into formic acid and NaH
2PO
4--the compound phosphoric acid sodium salt.Formic acid steams the finished product formic acid (concentration＞85%) that condensation is recycled into higher concentration, NaH
2PO
4--the compound phosphoric acid sodium salt can be used for making various sodium phosphate salts.
2 by the described method of claim 1, and it is characterized in that: peroxophosphoric acid can be a direct production; Also can be the lower concentration phosphoric acid inspissation of producing with hot method, wet method and additive method.
3 by the described method of claim 1, it is characterized in that: sodium formiate can be with yellow phosphoric tail gas and caustic soda synthetic; It also can be the sodium formiate of producing with additive method.
4 by the described method of claim 1, it is characterized in that: peroxophosphoric acid and the reaction of sodium formiate mixing, can in reactor, carry out, and also can in the formic acid distillation still, directly carry out.
5 by the described method of claim 1, it is characterized in that: in peroxophosphoric acid and the sodium formiate mixing reaction process, can return and throw small part formic acid; Also can not return input formic acid.The mixing reaction can be carried out at normal temperatures, also can carry out under less than the comparatively high temps of formic acid boiling point, and total mixing reaction times is 1～8h; Always steam formic acid time 2～8h.Mixing reaction and distillation (formic acid) can periodical operation; Also can operate continuously.
6 by the described method of claim 1, it is characterized in that: the NaH of by-product
2PO
4--compound phosphoric acid sodium can be directly used in the raw materials for production of Sodium hexametaphosphate 99; Also it can be handled through methods such as phosphoric acid, alkali (soda ash, caustic soda) heating, be used to make one, two, three, four, five sodium phosphate salts and other compound phosphoric acid sodium salts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103209A CN1066132C (en) | 1997-03-18 | 1997-03-18 | Method for producing formic acid and coproducing various phosphates by acidifying sodium formate with perphosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103209A CN1066132C (en) | 1997-03-18 | 1997-03-18 | Method for producing formic acid and coproducing various phosphates by acidifying sodium formate with perphosphoric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1179413A true CN1179413A (en) | 1998-04-22 |
| CN1066132C CN1066132C (en) | 2001-05-23 |
Family
ID=5166573
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97103209A Expired - Lifetime CN1066132C (en) | 1997-03-18 | 1997-03-18 | Method for producing formic acid and coproducing various phosphates by acidifying sodium formate with perphosphoric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1066132C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362682B (en) * | 2008-09-23 | 2011-02-09 | 余华强 | Method for producing formic acid with joint production of sodium phosphate by peroxyphosphoric acid and sodium formate |
| CN101665423B (en) * | 2009-08-11 | 2012-11-21 | 绵阳启明星磷化工有限公司 | Method for preparing methanoic acid by potassium formate acidized by phosphoric acid |
| CN102951625A (en) * | 2011-08-25 | 2013-03-06 | 贵州省惠水磷酸盐厂 | Sodium pyrophosphate preparation technology |
| CN105084335A (en) * | 2014-05-12 | 2015-11-25 | 天津市碳一有机合成工程设计有限公司 | Cogeneration method for producing monopotassium phosphate and potassium diformate |
| CN106241767A (en) * | 2016-08-29 | 2016-12-21 | 武汉东晟捷能科技有限公司 | A kind of method preparing potassium dihydrogen phosphate |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100540520C (en) * | 2007-08-24 | 2009-09-16 | 宜宾天原集团股份有限公司 | The method for preparing formic acid with phosphoric acid extraction and sodium formiate |
| CN101475463B (en) * | 2009-01-21 | 2011-09-21 | 曹勇 | Method for coproduction of high purity aminic acid and acid sodium phosphate by reaction of calcium formate and peroxyphosphoric acid |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE309412B (en) * | 1964-04-03 | 1969-03-24 | Perstorp Ab | |
| DE3137356C2 (en) * | 1981-09-19 | 1984-04-05 | Davy McKee AG, 6000 Frankfurt | Process for the production of concentrated formic acid |
-
1997
- 1997-03-18 CN CN97103209A patent/CN1066132C/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362682B (en) * | 2008-09-23 | 2011-02-09 | 余华强 | Method for producing formic acid with joint production of sodium phosphate by peroxyphosphoric acid and sodium formate |
| CN101665423B (en) * | 2009-08-11 | 2012-11-21 | 绵阳启明星磷化工有限公司 | Method for preparing methanoic acid by potassium formate acidized by phosphoric acid |
| CN102951625A (en) * | 2011-08-25 | 2013-03-06 | 贵州省惠水磷酸盐厂 | Sodium pyrophosphate preparation technology |
| CN105084335A (en) * | 2014-05-12 | 2015-11-25 | 天津市碳一有机合成工程设计有限公司 | Cogeneration method for producing monopotassium phosphate and potassium diformate |
| CN106241767A (en) * | 2016-08-29 | 2016-12-21 | 武汉东晟捷能科技有限公司 | A kind of method preparing potassium dihydrogen phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1066132C (en) | 2001-05-23 |
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