CN106829898A - A kind of method that utilization TMAH mother liquor prepares Arizona bacilli - Google Patents
A kind of method that utilization TMAH mother liquor prepares Arizona bacilli Download PDFInfo
- Publication number
- CN106829898A CN106829898A CN201710013116.2A CN201710013116A CN106829898A CN 106829898 A CN106829898 A CN 106829898A CN 201710013116 A CN201710013116 A CN 201710013116A CN 106829898 A CN106829898 A CN 106829898A
- Authority
- CN
- China
- Prior art keywords
- mother liquor
- tmah
- arizona bacilli
- utilization
- prepares
- 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.)
- Pending
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/163—Phosphorous acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method that utilization TMAH mother liquor prepares Arizona bacilli, using calcium chloride, phosphorous acid mother liquor and TMAH mother liquor for raw material carries out synthesizing prepared Arizona bacilli.It is an advantage of the invention that：Obtained Arizona bacilli sulfuric monohydrate is easily dried and product purity is high.In addition, the method has also reached the purpose to the purification of TMAH mother liquor while Arizona bacilli is produced.Meanwhile, the yield of the technique is very high, and the conversion ratio of calcium chloride can reach 100%.
Description
Technical field
The present invention relates to a kind of preparation method of Arizona bacilli, specifically, it is related to one kind to utilize TMAH
The method that mother liquor prepares Arizona bacilli.
Background technology
Arizona bacilli is widely used in paint industry as the nontoxic difunctional rust resisting pigment of one kind.Arizona bacilli
Preparation generally with ammoniacal liquor or NaOH as alkaline reactant, because the alkalescence of ammoniacal liquor is too weak, influence reaction efficiency and product
The purity of product；And drying is difficult using the moisture in aqueous Arizona bacilli obtained in NaOH, and side product chlorinated sodium is easy
Sodium chloride is not easy removal totally in deliquescence, the aqueous solution.For this reason, it may be necessary to a kind of new technical scheme is asked solving above-mentioned technology
Topic.
The content of the invention
It is an object of the invention to provide a kind of method that utilization TMAH mother liquor prepares Arizona bacilli, the method
Obtained Arizona bacilli sulfuric monohydrate is easily dried and product purity is high.In addition, the method is while Arizona bacilli is produced
Also the purpose to the purification of TMAH mother liquor has been reached.
The technical solution adopted by the present invention：
A kind of method that utilization TMAH mother liquor prepares Arizona bacilli, it utilizes calcium chloride, phosphorous acid mother liquor and four
Ammonium hydroxide mother liquor carries out synthesizing prepared Arizona bacilli for raw material.Specifically preparation process is：Phosphorous acid mother liquor is made into 10
~60% aqueous solution, and add reactor, then it is slowly added into calcium chloride and is reacted, added after 5~50 minutes and measure
And TMAH mother liquor that be diluted to 15~35%；Question response terminate after by the hydrate of gained solid phosphorous acid calcium one
Thing is filtered out, and the remaining aqueous solution carries out electrolytic preparation and obtains tetramethylammonium hydroxide aqueous solution.
The calcium chloride is 1.3~7.7 with the mass ratio of phosphorous acid mother liquor:1.
The TMAH mother liquor is 4.6~10.2 with the mass ratio of calcium chloride:1.
The reaction temperature control is at 40~80 DEG C.
It is an advantage of the invention that：Obtained Arizona bacilli sulfuric monohydrate is easily dried and product purity is high.In addition, the party
Method has also reached the purpose to the purification of TMAH mother liquor while Arizona bacilli is produced.Meanwhile, the receipts of the technique
Rate is very high, and the conversion ratio of calcium chloride can reach 100%.
Specific embodiment
Embodiment 1
By in 10% phosphorous acid mother liquor addition reactor, then it is slowly added into calcium chloride and is reacted, calcium chloride is female with phosphorous acid
The mass ratio of liquid is 7.7:15% TMAH mother liquor, TMAH mother liquor and chlorination are added after 1,5 minute
The mass ratio of calcium is 4.6:1；Question response filters out gained solid phosphorous acid calcium sulfuric monohydrate after terminating, remaining water-soluble
Liquid carries out electrolytic preparation and obtains TMAH, and whole reaction temperature control is at 40~80 DEG C.
After testing, purity is 99.2% to obtained Arizona bacilli product.
Embodiment 2
By in 60% phosphorous acid mother liquor addition reactor, then it is slowly added into calcium chloride and is reacted, calcium chloride is female with phosphorous acid
The mass ratio of liquid is 1.3:35% TMAH mother liquor, TMAH mother liquor and chlorine are added after 1,50 minute
The mass ratio for changing calcium is 10.2:1；Question response filters out gained solid phosphorous acid calcium sulfuric monohydrate after terminating, remaining
The aqueous solution carries out electrolytic preparation and obtains TMAH, and whole reaction temperature control is at 40~80 DEG C.
After testing, purity is 99.25% to obtained Arizona bacilli product.
Embodiment 3
During 40% phosphorous acid mother liquor added into reactor, then it is slowly added into calcium chloride and is reacted, calcium chloride and phosphorous acid
Mass ratio is 1.5:25% TMAH mother liquor, TMAH mother liquor and calcium chloride are added after 1,30 minute
Mass ratio be 8.2:1；Question response filters out gained solid phosphorous acid calcium sulfuric monohydrate after terminating, the remaining aqueous solution
Carry out electrolytic preparation and obtain TMAH, whole reaction temperature control is at 40~80 DEG C.
After testing, purity is 99.35% to obtained Arizona bacilli product.
Claims (5)
1. a kind of method that utilization TMAH mother liquor prepares Arizona bacilli, it is characterised in that：Using calcium chloride, phosphorous
Acid mother liquor and TMAH mother liquor carry out synthesizing prepared Arizona bacilli for raw material.
2. the method that a kind of utilization TMAH mother liquor according to claim 1 prepares Arizona bacilli, its feature
It is：Specifically preparation process is：Phosphorous acid mother liquor is made into 10~60% aqueous solution, and adds reactor, then slowly plus
Enter calcium chloride to be reacted, TMAH mother liquor that is measuring and being diluted to 15~35% is added after 5~50 minutes；
Question response filters out gained solid phosphorous acid calcium sulfuric monohydrate after terminating, and the remaining aqueous solution be electrolysed obtaining tetramethyl
Base ammonium hydroxide aqueous solution.
3. the method that a kind of utilization TMAH mother liquor according to claim 1 and 2 prepares Arizona bacilli, it is special
Levy and be：The calcium chloride is 1.3~7.7 with the mass ratio of phosphorous acid mother liquor:1.
4. the method that a kind of utilization TMAH mother liquor according to claim 1 and 2 prepares Arizona bacilli, it is special
Levy and be：The TMAH mother liquor is 4.6~10.2 with the mass ratio of calcium chloride:1.
5. the method that a kind of utilization TMAH mother liquor according to claim 1 and 2 prepares Arizona bacilli, it is special
Levy and be：The reaction temperature control is at 40~80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710013116.2A CN106829898A (en) | 2017-01-09 | 2017-01-09 | A kind of method that utilization TMAH mother liquor prepares Arizona bacilli |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710013116.2A CN106829898A (en) | 2017-01-09 | 2017-01-09 | A kind of method that utilization TMAH mother liquor prepares Arizona bacilli |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106829898A true CN106829898A (en) | 2017-06-13 |
Family
ID=59118048
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710013116.2A Pending CN106829898A (en) | 2017-01-09 | 2017-01-09 | A kind of method that utilization TMAH mother liquor prepares Arizona bacilli |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106829898A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1523135A (en) * | 2003-02-18 | 2004-08-25 | �Ͼ���ҵ��ѧ | Process for preparing tetramethyl ammonium hydroxide by electrolysis-electrodialysis |
| CN102206832A (en) * | 2011-04-29 | 2011-10-05 | 郑州大学 | Method for preparing electronic-grade tetramethylammonium hydroxide (TMAH) |
| CN103058156A (en) * | 2011-10-18 | 2013-04-24 | 王军民 | Method for preparing calcium phosphate by utilizing slag charge discharged during sodium hypophosphite preparation |
| CN103723696A (en) * | 2014-01-10 | 2014-04-16 | 杨洋 | Preparation method of calcium phosphite |
| CN104936891A (en) * | 2012-04-06 | 2015-09-23 | 罗地亚经营管理公司 | Process for production of hypophosphite salts |
-
2017
- 2017-01-09 CN CN201710013116.2A patent/CN106829898A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1523135A (en) * | 2003-02-18 | 2004-08-25 | �Ͼ���ҵ��ѧ | Process for preparing tetramethyl ammonium hydroxide by electrolysis-electrodialysis |
| CN102206832A (en) * | 2011-04-29 | 2011-10-05 | 郑州大学 | Method for preparing electronic-grade tetramethylammonium hydroxide (TMAH) |
| CN103058156A (en) * | 2011-10-18 | 2013-04-24 | 王军民 | Method for preparing calcium phosphate by utilizing slag charge discharged during sodium hypophosphite preparation |
| CN104936891A (en) * | 2012-04-06 | 2015-09-23 | 罗地亚经营管理公司 | Process for production of hypophosphite salts |
| CN103723696A (en) * | 2014-01-10 | 2014-04-16 | 杨洋 | Preparation method of calcium phosphite |
Non-Patent Citations (1)
| Title |
|---|
| 徐旺生等: "亚磷酸氢钙生产工艺研究", 《武汉化工学院学报》 * |
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| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170613 |
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| RJ01 | Rejection of invention patent application after publication |