CN1088455C - Preparation of sodium salt solution of methyl benzotriazazole - Google Patents
Preparation of sodium salt solution of methyl benzotriazazole Download PDFInfo
- Publication number
- CN1088455C CN1088455C CN99114136A CN99114136A CN1088455C CN 1088455 C CN1088455 C CN 1088455C CN 99114136 A CN99114136 A CN 99114136A CN 99114136 A CN99114136 A CN 99114136A CN 1088455 C CN1088455 C CN 1088455C
- Authority
- CN
- China
- Prior art keywords
- sodium salt
- methyl benzotriazazole
- methylbenzotriazole
- methyl
- salt solution
- 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.)
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- 159000000000 sodium salts Chemical class 0.000 title claims abstract description 19
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 title claims description 23
- 239000012266 salt solution Substances 0.000 title claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 23
- 238000010189 synthetic method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- RPKCLSMBVQLWIN-UHFFFAOYSA-N 2-n-methylbenzene-1,2-diamine Chemical compound CNC1=CC=CC=C1N RPKCLSMBVQLWIN-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 abstract 5
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 abstract 4
- 235000010288 sodium nitrite Nutrition 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000003112 inhibitor Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- BMOKHTQIBPRXSL-UHFFFAOYSA-N 2h-benzotriazole;sodium Chemical compound [Na].C1=CC=CC2=NNN=C21 BMOKHTQIBPRXSL-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 239000000243 solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Plural Heterocyclic Compounds (AREA)
Abstract
The present invention relates to a synthetic method for the sodium salt of methylbenzotriazole, which is widely applied to metal antirusting agents and metal corrosion inhibitors. The synthetic method comprises the steps: methyl-o-phenylenediamine and excessive sodium nitrite are used as main raw materials and react at a certain temperature and a certain pressure to synthesize the sodium salt of methylbenzotriazole in one step, or methylbenzotriazole and sodium hydroxide react to prepare the sodium salt of methylbenzotriazole. The synthesis temperature of the present invention is from 180 DEG C to 280 DEG C, the pressure is from 22 kg/cm<2> to 60 kg/cm<2>, and the molar ratio of the methyl-o-phenylenediamine to the sodium nitrite is 1:1 to 1.5. The sodium salt of methylbenzotriazole, which is produced by using the method, has the advantages of low production cost, large dissolvability in water and convenient application.
Description
The present invention relates to a kind of synthetic method that metal plays the methyl benzotriazazole sodium salt solution of antirust, inhibition and antioxygenation that is applied to.
The existing metallic surface that acts on is played the rust-preventive agent of antirust, inhibition and antioxygenation methyl benzotriazazole and benzotriazole sodium salt etc. is arranged.Methyl benzotriazazole though its price is lower, is used cumbersome because the solubleness in water is little.Though and its solubleness in water of benzotriazole sodium salt is very big, its synthetic main raw material O-Phenylene Diamine price height, 2.2 ten thousand yuan/ton, manufacturing cost is higher.The price of benzotriazole sodium salt is above 30,000 yuan.Though it is of many uses and difficult is accepted and applies by the user.
The object of the present invention is to provide a kind of synthetic method of the methyl benzotriazazole sodium salt solution that the big production cost of solubleness is low again in water.
The present invention is achieved in that a kind of synthetic method of methyl benzotriazazole sodium salt solution, and it is to make the methyl benzotriazazole sodium salt solution with methyl benzotriazazole and sodium hydroxide reaction, and its reactions steps is:
Because methyl benzotriazazole sodium salt manufacturing process, physico-chemical property and application performance and its like product benzotriazole sodium salt are similar, and the byproduct that its main raw material methyl-o-phenylenediamine is TDI, MDI, price is low, 0.8 ten thousand yuan/ton, the main raw material O-Phenylene Diamine price height of benzotriazole sodium salt, 2.2 ten thousand yuan/ton, so the production cost of methyl benzotriazazole sodium salt is low than the benzotriazole sodium salt, in majority is used, substitute benzotriazole, apply and to reduce user cost greatly.After this product made 99% solid, be convenient to long-distance transport, reduce expenses.This product and water dissolve each other, and the solubleness in water is very big, need not increase any equipment or technology in application units, as long as directly add, use easily.
Fig. 1 is a process flow sheet of the present invention.
Below in conjunction with accompanying drawing the present invention is made a detailed description:
The present invention is a kind of synthetic method of methyl benzotriazazole sodium salt solution.The methyl benzotriazazole sodium salt is widely used in the rust-preventive agent and the buffer reagent of metal.It is to make the methyl benzotriazazole sodium salt solution with methyl benzotriazazole and sodium hydroxide reaction, and its reactions steps can be write as:
Wherein sodium hydroxide (sheet alkali) content is more than 96%, below the cl content 50ppm.
Embodiment 1: in there-necked flask, throw 45 parts of (weight) methyl benzotriazazoles, adding alkali lye (15 parts in sheet alkali and 45 parts＜weight of water 〉), 50 ℃ were stirred 3 hours, add 80 parts of water dilutions and add 5 parts of gacs again, stir 3h, be as cold as 30 ℃, filter with B, filter cake is with the drip washing of 70 parts of moisture secondaries.Filtrate is inspissation in 2 liters of there-necked flasks, and 103～114 ℃ through 3～4h, steams about 100 parts of water, 100 parts of solution, content is about 50%, yield 95% is golden yellow or yellowish brown transparent liquid.
Embodiment 2: the 145kg deionized water is thrown in the 1000L reactor of heating jacket is arranged, dissolved fully in 60 ℃ of stirrings.In above-mentioned reactor, drop into the 440kg methyl benzotriazazole,,, add the 10kg gac, stirred filtration 3 hours if the color is too dark in about 1 hour of 50 ℃ of left and right sides stirring and dissolving.Analyze content and pH value, it is qualified that water or liquid caustic soda solution are adjusted to.Get 50% methyl benzotriazazole sodium salt solution 1000kg.
After this product made 99% solid, be convenient to long-distance transport, reduce expenses.
This product and water dissolve each other, and the solubleness in water is very big, do not need to add any equipment or technology in application units again.As long as directly add, use easily.
This product can be made into 40%, 50%, 60%, 70% isocyatic solution as required.
Claims (2)
1, a kind of synthetic method of methyl benzotriazazole sodium salt solution is characterized in that it is to make the methyl benzotriazazole sodium salt with methyl benzotriazazole and sodium hydroxide reaction, and its reactions steps is:
2, the synthetic method of a kind of methyl benzotriazazole sodium salt solution according to claim 1 is characterized in that the sodium hydroxide that reacts with methyl benzotriazazole is sheet alkali, and content is more than 96%, below the cl content 50ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99114136A CN1088455C (en) | 1999-03-27 | 1999-03-27 | Preparation of sodium salt solution of methyl benzotriazazole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99114136A CN1088455C (en) | 1999-03-27 | 1999-03-27 | Preparation of sodium salt solution of methyl benzotriazazole |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1235161A CN1235161A (en) | 1999-11-17 |
| CN1088455C true CN1088455C (en) | 2002-07-31 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99114136A Expired - Fee Related CN1088455C (en) | 1999-03-27 | 1999-03-27 | Preparation of sodium salt solution of methyl benzotriazazole |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1088455C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607946B (en) * | 2009-07-24 | 2012-01-25 | 南京神柏远东化工有限公司 | Method for purifying tolytriazole sodium salt |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100400520C (en) * | 2006-05-24 | 2008-07-09 | 河北沧州大化集团新星工贸有限责任公司 | Method for extracting methyl o-phenylenediamine from TDI organic residue and using it to synthesize TTA |
| CN102912353B (en) * | 2011-08-04 | 2014-09-17 | 上海泰禾化工有限公司 | Method for preparing tolyltriazole (TTA) sodium salt solution by utilizing TTA former fraction |
| CN103992282A (en) * | 2014-06-03 | 2014-08-20 | 如皋市金陵化工有限公司 | Production method of tolytriazole sodium salt |
| CN106086898B (en) * | 2016-08-20 | 2018-06-05 | 哈尔滨锅炉厂有限责任公司 | Volatile rust prevention powder of carbon steel and low alloy steel and preparation method thereof |
| CN108148008A (en) * | 2018-02-02 | 2018-06-12 | 肖志才 | A kind of production method of 4- methyl benzotriazazoles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04360879A (en) * | 1991-06-10 | 1992-12-14 | Mitsui Toatsu Chem Inc | Method for purifying aromatic triazoles |
| JPH04360878A (en) * | 1991-06-10 | 1992-12-14 | Mitsui Toatsu Chem Inc | Production of aromatic triazoles |
-
1999
- 1999-03-27 CN CN99114136A patent/CN1088455C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04360879A (en) * | 1991-06-10 | 1992-12-14 | Mitsui Toatsu Chem Inc | Method for purifying aromatic triazoles |
| JPH04360878A (en) * | 1991-06-10 | 1992-12-14 | Mitsui Toatsu Chem Inc | Production of aromatic triazoles |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607946B (en) * | 2009-07-24 | 2012-01-25 | 南京神柏远东化工有限公司 | Method for purifying tolytriazole sodium salt |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1235161A (en) | 1999-11-17 |
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