CN1088455C - Preparation of sodium salt solution of methyl benzotriazazole - Google Patents

Preparation of sodium salt solution of methyl benzotriazazole Download PDF

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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
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sodium salt
methyl benzotriazazole
methylbenzotriazole
methyl
salt solution
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CN1235161A (en
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徐道如
颜振兴
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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 synthetic method of methyl benzotriazazole sodium salt solution
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:
Figure C9911413600031
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:
Figure C9911413600041
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:
Figure C9911413600021
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.
CN99114136A 1999-03-27 1999-03-27 Preparation of sodium salt solution of methyl benzotriazazole Expired - Fee Related CN1088455C (en)

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CN1088455C true CN1088455C (en) 2002-07-31

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Cited By (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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-phenylendiamine from TDI organic residue and synthesizing TTA using same
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04360879A (en) * 1991-06-10 1992-12-14 Mitsui Toatsu Chem Inc Purification of aromatic triazoles
JPH04360878A (en) * 1991-06-10 1992-12-14 Mitsui Toatsu Chem Inc Production of aromatic triazoles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04360879A (en) * 1991-06-10 1992-12-14 Mitsui Toatsu Chem Inc Purification of aromatic triazoles
JPH04360878A (en) * 1991-06-10 1992-12-14 Mitsui Toatsu Chem Inc Production of aromatic triazoles

Cited By (1)

* Cited by examiner, † Cited by third party
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

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