SU474971A4 - Method for producing ethylene unsaturated beta-hydroxy ester - Google Patents

Description

The TCMnepaiyipe environment has been in place for more than 28 weeks without any reduction in the health of a: KT111vats1ni 1a affected by iiiiiiCM HOttii3HipyiOLuero radiation.

The number of tin salts of tin salts that can be applied is different from those of halogen free waves, like tin dichloride (SnCl 2). The amount of tin, introduced into the reaction tank, can vary considerably, usually it should be approximately 0.10-1.0 times. %, echita on the number of reacting substances, deserving their participation in the formation of a complex e (|) world. More and more respectable amounts of Pribotizivno 0,2-0,6 weight. %, counting on. number of reagents.

Elite is unsaturated, Isoh :: ny (3-hydroxy: f), anti-nitrophic acid is added, and alkaline catalysts are used to reduce the amount of alkaline catalysts to reduce the amount of reagent. ammonium, benzyltri.methylproduct .i.ce hydrate, o-ucyiAmdshNI, K, M-di1methylaniJK ii, b, l - | benzyldi methylme-miN, potassium hydroxide or hydrate okti lithium.

The amount of catalyst incorporated into the reaction mixture may vary in 31 hectares of nutrients. It should ordinarily be about 0.2-2.0 1 weight. % nrel | respectfully 0.6-0.8 wt. %, counting on the amount of the reaction of C dich substances.

The reaction and the production of an unsaturated p-hydroxyether, stable IK gel formation, is carried out in 1P (dissolving or dissolving day; TILENTS or without them. Ed-d and re-elucidating substances are FID1K) OTHER, then the reactionC (you can do it), and the resolving agents are FID) KO, then the reaction (you can do it). in the absence of solvents.

In cases where the hell is about ilm, both reacting substances are I1 solid solids, and it is advisable to add a solvent in order to improve the quality of the reaction: C: C; C; I | I. Primarol n paihnyh solvents. Molol Serve ketones, - a measure of methyl methyl ethyl ketone, hydrocarbons, i-1nri: IU, p da 11kloteyus1n, and aramatne-chekne solutionstrels, for example, toluene “pp.

The reaction of the formation of the p-hydroxyether usually is 1: 1; water or ir C is: preferably 90-105 ° C. The reaction is carried out in an inert atmosphere such as nitrogen. Further, the reaction, we can, but moral at atmospheric or nokizhennom pressure with a reversible refrigerator.

It takes 1-10 hours to complete, resulting in the formation of the p-axiater. The same time is required for the complete consumption of unsaturated 5: arboxylic acid. The progress of the relay is easy to control by identifying the joints. It is believed that the reaction is essentially complete if the ki1Slot1NO1St has gone to 1 acid number of 10 or less.

Upon completion of the formation of the p-hydroxy ester, if necessary, the olo salt can be disactivated with the 1 lucent of the target ester, and treated with 85-95% phosphoric acid. For deacidification salt, the acid is added to the product of the reaction with a mixture of ester and ester to obtain a concentration of 0.1-0.2 weight. %, based on the amount of ester, and the mixture is allowed to grow up to 25-40 ° C for 0.5-2 hours, after which the insoluble colloidal solid can be separated from the product by the reaction. Another uncomplicated method of separation can be used for the separation, or it can be left as part of the reaction product.

The relationship between ethylenically unsaturated α, β-carbonic acid and nolipo | SidO | M, iridescent. tions and oleaginous unsaturated COMPLEX p-oxyeff | ira l containing its compounds, is not of particular importance. In general, 1-2 molar equivalents of non-amino carboxylic acid are used per 1 molar equivalent of patioeoxide.

Acrylic acid, methacrylic acid and crotonic acid are used as ethylene a, p-unsaturated carboxylic acids having 3-6 carbon atoms. Among these acids, acrylic acid and: methacrylate kislot are preferred. In the manufacture of complex p-oxyether, a part of the y-ohm of saturated unsaturated acids can be replaced by saturated acids containing 3-18 carbon atoms, like capril, pelaric carbon, palmitic, and similar, with the goal of variating the physical properties of complex p - caaether. Saturated Acid is CAN (TURNED into a reaction medium at a concentration that should not exceed 25 mol.%, Considering the total quantity of acid. Usually the amount of saturated acid added is 5-20 mol.%.

Polyepioids, used to produce p-o-esters, include organic compounds, the molecule of which contains at least two reactive epoxy groups,

,

those. (1V, -npytninbi. Polyepoxides are supposed to be Saturated or unsaturated, aliphatic: cycloaliphatic, aromatic and / or heterocyclic; CMI and can be replaced by substituents.

Aromatic 1-to-1 epoxy are polymeric products of the reaction, produced by: between a plurality of one and one and the other: polyphenol and polyphenol (and halohydrite: by us and / or glycerol dichlorohydrin.

A typical aromatic agent, m poly (1) polyoxy, is a reaction product of the interaction of amp; p) hydrochloride acid with 2.2-b "c- (p-1C1Cypheelnyl) propyne (Bisphenol A), a resin, the following structural formula:

 L

N., 0-OI-S 1 - | 0

where n is equal to 0 or cslo.m number up to 10.

Values should not exceed 2 or 3, 1 or less:: Less.

Aliphatic polyapoicides are: 1 || -methylene glycol, tetra a | Methyl anglicol, these l en ch icol, polyethyl leclycol, poltgbutylevglnkol and similar

I1M.

The stabilized ethylenically unsaturated p-axion ester and the compositions based on it have been proposed according to the proposed method; they are useful and suitable materials for the manufacture of a coating that can be cured under the effect of radiation. Such a coating can be applied on the most diverse materials, judging asnavoy or substrate, including metal, paper and wood. The stabilized ester can be used either as such or in combination with other ns-saturated compounds such as vinyl monomers and the like.

Stable waxy complex | 3-oocyte profiles are particularly suitable as components of bonding materials for printing and printing inks that can be cured by ultraviolet radiation. In the manufacture of such binders for printing inks, stabilized, ethylenically unsaturated 3-hydroxyether, it is advisable to mix with one, at least, ethylenically unsaturated COMPLEX polyether, such as polyacrylates and polyitonates, as well as with a photosensitizer.

Example 1. In a reactor equipped with konOpyt I Stabilizer

j SnC,

Claims (4)

I is missing The reaction product is gelated. during synthesis SrCi, Catalyst not lrmms.n ln CuCb The reaction product gelled during the synthesis. ZnCl, an acid number of 163 indicates that the consensus is not included in the reaction. HE-, l (Vo-OHjOH-CH, SI 3 400 g (1.15 mol) of bisphenol A - diglycidyl ether, 132.8 g (1.84 mol of glacial acrylic acid, 4.0 g of benzyl dimethylamine, 2 , 0 g dvuhlorort Stoboy (, in the form of a solution in 50 ml of methyl ethyl ketone). The teleshutory of the reaction mixture} increases and maintains at about 102 ° C for 4.0 hours 0 iB nitrogen atmosphere. Titration of the sample reaction mixture of 0.2 n. using a potassium hydroxide solution of potassium oxide, carried out with this thromhiji, showed that the reaction has an acid number of 1.4. This suggests that the reaction between the bisphenol ether and acrylic acid is substantially completely melted. The resulting reaction product is a yellowish, slightly turbid solution. The reaction mixture, the soda, the neighing mixture of the bisphenolic ether with acrylic acid ester, is then treated with 1 g of 86.7% orthophosphoric acid in 100 ml of methyl ethyl ketone and stirred for 1 hour at room temperature; in order to deactivate the two-halogen tin and neutralize it for 1 hour at room temperature; catalyst. Part of decontamination: 31 rosane reaction mixtures are placed in a brown glass jar and systematically checked for the presence of a gel. Indicators of the stability of the gel are given IB table. D.LA comparison, a separate series of reactions is repeated, using the npiHiMepa 1 method, but also dichloride tin or not note the catalyst in the form of benzyldimethyl: on, or a different metal chloride salt is added to the reaction mixture than dichloride tin. These comparative formulations are also tested for the stability of g, l. These experiments are indicated by IB Table 2-5. Waloychkppst Results on a b gel, nedelm The same amount of acrylic Example 2. Example 1 is repeated, but the reaction product containing the complex (3-hydroxyether is not treated with phosphoric acid. Gel formation was noted after storing the reaction product containing the ester in a brown glass vessel for more than 3 months . Subject invention . The method of obtaining ethylene non-purported complex p-oxiphir by means of a, p-unsaturated carboxylic acid containing 3-6 carbon atoms, with a polyepocoid in an alkaline catalyst and stabilizer of the target product with the next product; techniques, characterized in that, in order to obtain a tar of an article that is stable against the ischemia of the gel and which is similar to polymerization under the action of ionizing radiation, a tin halide salt is used as a stabilizer. 2. Method 1, characterized in that Bisphenol A diglycid ether is taken as poly (ethylene) oxide; 3.Styuzob lo n. 1, characterized in that the salt is halogen-free; water, Sn / 2, does not contain SnCl2 with a concentration in the reaction mass equal to 0.1 -1.0 wt.%. 4. A method according to claim 1, characterized in that a tertiary amine is used as an alkaline catalyst, for example K, X-benzyldimethylamine. Priorities by featured: 04/10/22 when used as catalysts of amps and tin salts iB as stabilizer of the target product; 11/13/72 with the use of alkali alkaline catalysts and olea halide salt as a stabilizer of the desired product.