JPS5869841A - Stabilizer for hydroxylamine - Google Patents

Abstract

PURPOSE:A stabilizer stabilizing hydroxylamine by the addition of its small amount, not crystallizing a reaction inhibitor such as Na2SO4, etc., usable in a state of a concentrated solution, comprising a specific 1,10-phenanthroline. CONSTITUTION:A stabilizer comprising a 1,10-phenanthroline shown by the formulaI(R is H, lower alkyl, halogen, or phenyl) such as 1,10-phenanthroline, 5- methyl-1,10-phenanthroline, 5-chloro-1,10-phenanthroline, 5-phenyl-1,10-phenanthroline, etc. The number of moles of the stabilizer is 0.001 based on that of hydroxylamine. Stabilized hydroxylamine and its salts are useful for fiber treatment, dyeing process, natural color photograph, rubber industry, oil and fat industry, synthesis for drugs and agricultural chemicals, a raw material for organnic synthesis, etc. EFFECT:When it is used in a reaction, it has merits such as increase in capacity by the same device, the rationalization of the power of man and process, etc.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a stabilizer for 1-10-phenanthroline represented by the following general formula.

Human ■ Yasiluain and its salts prevents oxidation.

It is used in delicate processing, dyeing industry, natural color photography, rubber industry, oil and fat industry, Okibe synthesis, agricultural chemical synthesis, etc.In recent years, especially as the geological formations as raw materials for organic synthesis have increased to 19%, hydrosilane has a melting point of 33. 05G is an extremely unstable base, and its 4.06 Mot/L aqueous solution showed 79.7% decomposition when kept at 40C for 144 hours9.
However, the aqueous solution of the salt is extremely stable, sMot/L, 50
C. Decomposition was within the measurement error even after one month of standing. Therefore, it is commercially available as a stable sulfate, hydrochloride, or nitrate. However, many of these applications do not require hydroxyl azanosalts, but rather hydroxylamine salts. At present, the substance is neutralized with an alkali in a solvent containing the substance and then used as an aqueous solution.

Reaction #III& generally uses an organic solvent such as arbules. That is, the substance to be reacted is dissolved in a solvent, crystals of fluorine, for example, are added to the solution in hydrosulfuric acid, stirred, and an alcoholic solution containing NaOH is gradually added to cause the solution to warp. In this case, a film of Na1804 of mold Im crystals which is insoluble in solid human gastric sulfuric acid l[Kal=-l] is formed, and Na0HO alcohol *
* prevents @ from reaching the crystals of human tetraxylamine sulfate. And at the end of the reaction, unused sulfuric acid human WI is covered with a thick Na1804 film? Silurian particles remain. In actual factory operations, the number of unused sulfuric acid molecules can reach as high as 101. Furthermore, in order to prevent pollution, it becomes necessary to oxidize and remove this unused material using an oxidizing agent.

In addition, at the end of the reaction, nine molds were produced during the alcohol fII reaction.
Due to the crystals of 11 Na, 8o4, the entire reaction solution becomes porridge-like, and the loss of the active ingredient during removal of the crystals is also large. It is almost the same even if human tetraxylamine hydrochloride or human tetraxyl nitrate (y) is used instead of human tetraxylamine sulfate.

The present invention provides stable human tetraxylamine by adding a 1-10-7 enanthrolytic stabilizer. 10-phenanthaterite is hydroxylua $
3104# Only 1/1,000 to 1/10,00 of the number
By only containing 0x, hydrosilane is kept extremely stable with almost no public records.

Furthermore, according to the present invention, by using stable human tetraxylamine in the reaction? ), NIL! 80. Because it does not crystallize reaction inhibitors such as, it is possible to carry out the reaction by Takatsuhama. Since crystals such as N also, etc. do not crystallize, centrifugation can be eliminated, eliminating loss of reaction products and liquids. Therefore, the same equipment has many advantages such as increased capacity and rationalization of manpower and processes.

Next, examples will be shown.

Example 1 JIB K8995 sulfuric acid hydroxyl reagent special grade is dissolved in pure water KfII to prepare approximately 5 Mot/L II solution.

This is called liquid A. Dissolve JIB K8576 special grade NaOH reagent #1 in pure water to make a solution of about 50%. This is designated as B11E. Next, the KA solution is cooled to 5GK and neutralized with the D solution previously cooled to 50GK. Neutralize with OC without stirring strongly.
~10C, and complete neutralization according to JIS z88
02o glass electron m method! jJllllffflL, PHa5
was the end point. After neutralization, cool the liquid to OC and Nap
so, e IQ 0 ink is precipitated, Planar-1
It was filtered using a filter paper. This is called liquid C.

As a result of measuring hydroxylamine in liquid C using the test method of JIS K8993, human tetraxylamine was 4.0.
It was 6MoL/L.

Cil was used as a stock solution, and to this was added various 1-10-phenates, which are the stabilizers of the present invention, each in an amount of 1 mol (1 liter) of hydroxyl Vluaden (1001 times the number of 4 mol). .

The amount of residual mid-12dP siluran was measured after being left at 40C for 6 hours, 16 hours, and 24 hours. The results were as shown in Table 1.

Example 2 JIB K8201 human tetraxylamine hydrochloride was dissolved in methyl alcohol to saturation at 40C (approximately 2
．． 75 Mol/L). This is called liquid D. Example 1
About 5 Mat/L of NaOH in methyl alcohol
It was dissolved so that This was used as liquid E. Next, liquid D was cooled to 5C, and liquid 1 was gradually added thereto while stirring vigorously and being careful not to let the liquid temperature exceed 10C. Then, a large amount of fine NaCL crystals are generated, and the liquid becomes porridge-like. Neutralization was measured using a glass electrode in the same manner as in Example 1, and the end point was set as PHa5. After neutralization, the filter paper was filtered through a Shiitomo P7ner funnel. This filtrate is designated as F solution. The content of toromozylamine in the F solution was measured in the same manner as in Example 1 and was found to be 1.98 MoL/L M 6 .

Next, Solution F was concentrated in a round-bottomed flask under reduced pressure at about 30C to approximately double the concentration. As a result of measurement in the same manner as in Example 1, the content of human tetraxylamine was 4.09 Mot.
It was JL. This is called liquid G.

G1ml was used as a stock solution, and various 1-10-zeneryl) lolines, which are i-fixing agents of the present invention, were added thereto in an amount of 1/10,000 moles of hydroxylamine. The test was then carried out in the same manner as in Example 1.

The results were as shown in Table 2.

Example 5 The difference from Example 2 was that ethyl alcohol was used as the solvent instead of ethyl alcohol, and the temperature was lowered at the dead center.

The rest is almost the same as the second embodiment. However, because of the poor solubility of human maP silua hydrochloride to ethyl allium i, the concentration of human xyzyl atom before the first contraction was a little thinner, and therefore the deformity was slightly increased. It was 96 MoL/L. Then, it was tested in the same manner as in Example 1, and the result was 1lI3.

Example 4 The only difference from Example 1 was the neutralization point. One of the two types of samples is PH&O, Hydroxylua Hyokun Noshi 4.00 H
ot/L-1” I C1 and others are PH7,0, human*
The QVk power flow rate was 4.05 MoL/L. Then, a 24-hour release test was conducted in the same manner as in Example 1, and the results were as shown in Table 4. For comparison, a portion of the results of Example 1 were also reproduced.

4 Example 5 The difference from Example 1 was that 50 sachets of an aqueous solution of cyamine (iris) was used in the distillation and sludge, the stabilizer was used at a concentration 104 times the number of moles of toxyl iso, and the test temperature was changed. is set to 55C. The following two types with the best stabilizer lines were selected and subjected to a long-term storage test of 100 to 680 hours (2x3 days).

The result was like 1lI5.

Example 6 The difference from Example 5 was that the humming test temperature was higher than 55C and 100C.
CKL9. The results were as shown in Table 6.

Claims (1)

[Claims] A stabilizer for hydroxyl iy consisting of 1-10-phenanthroline represented by the following general formula.