PL105171B1 - METHOD OF MAKING BAR AND CADMIUM STEARINATES AND LAURINATES - Google Patents

Description

The subject of the invention is a method for the production of steel barium-cadmium laurates and laurates, being non-dusting stabilizers for polyvinyl chloride, etc. chlorinated polymers.

Methods of making these stabilizers are known in an aqueous environment of soluble acid salts stea¬ rinse or lauric acid and soluble barium salts and cadmium, such as nitrates, chlorides, and sulfates, or in the reaction oxides or hydroxides of these metals and acids, for example cooked in the form of very fine suspensions, reacting in the presence of catalysts, e.g. of the amine type.

Salts of the mentioned carboxylic acids formed they fall out of the water in the form of very fine sediments, badly dripping and difficult to clean from arising by-products of mineral salts. They are very obese when dry fatty and dusty, which - due to their high toxicity possibility of explosion - creates many dangers swings.

Used as stabilizers in PVC processing due to the high degree of grinding and dustiness are cumbersome to pack and use because they are not suitable for automatic dosing continuously.

There are also known methods of making these stabilizers blockages by the fusion of oxides, hydroxide metals and carbonates with the corresponding carbohydrate xyls or their anhydrides.

In the case of the reaction with carboxylic acids, pro the process of obtaining the salt proceeds with unsatisfactory performance yield, and the product obtained is often unsuitable they are colored or contain unreacted oxides of metals, which in the case of the production of cadmium salts without performing additional, burdensome operations They can also be used as stabilizers. Salts obtained they are also often stretched or crumbly, no a homogeneous mass with a melting point higher than the softening point of PVC, which results in a poor they move and connect with the polymer ..

For improving the degree of reaction and recovery homogeneous product with the appropriate properties the stabilizers had to add a solvent that in addition, it lowered the temperature of the reaction and prevented thermal disintegration of the resulting salts.

In the case of obtaining these salts by the reaction of the oxides and metal hydroxides with carbohydrate anhydrides xyls it was necessary to use a large excess of meringue aquarius, which had to be then removed by extractions, for example with ether, or by distillation and elution no. The process itself took many hours days, at high temperatures of 80-250 ° C, because of this frequent thermal decomposition of higher anhydrides fatty acids. ' There is a known method of producing barium and cadmium salts in the reaction of these metal oxides and carboxylic acids in the environment of organic solvents, it is possible binders, azeotropic removal of water formed in reaction.

It was surprisingly found that stearates and laurates High quality barium-cadmium nannies, not available what disadvantages these stabilizers have, obtained according to methods of their production known so far, it is possible 105 171 105 171 to obtain the method according to the invention - by reaction of evil hydrogenation with brown cadmium oxide of acid stea gutter or lauric, used to create a suitable reaction environment - freely chosen most preferably a molar excess, in the presence of of the catalyst, such as hydrated sorbitol, and then used excess measure of stearic or lauric acid becomes more neutral a stoichiometric amount of octahydrate hydroxide in the presence of a drainage agent, they reduce the temperature of the reaction by lowering the temperature melting of the resulting stearate or ba- laurate of cadmium and allowing them to play at the same time lations or flaking, such as paraffin oil, paraffin, ethyl alcohol or glycerol monostearate, most more preferably paraffin oil.

The process of obtaining stearate or cadmium laurate speech may be conducted at a temperature of 100- 140 ° C with drainage under normal or reduced pressure. Produced stearates and barpwo-cadmium laurates are powdered, granulating or flaking. You get products non-dusty, with polychloride suitable for processing vinyl and other chlorinated polymers of temperature lower than the melting point of the polymer and with the required stabilizing and lubricating properties all.

The method of producing stearates and ba- laurates According to the invention, the tobacco-cadmium compounds according to the invention exceed those of more favorable conditions for them production and better quality of the products obtained ts as stabilizers.

The method of producing cadmium stearate or laurate in excess of stearic acid or lauric acid unlike previously known methods - enables - together with the catalyst used above, e.g. hydrated sorbitol - complete conversion of the brats cadmium oxide. barium-cadmium nanometers the percentage of barium Toxic metals such as barium and especially cadmium without the slightest reduction in their stabilizing properties; improves their lubricating properties and the ability to spread merging and merging with the mass of the polymer in the process of its transformation creativity and - which is extremely important - makes it possible to receive lack of dust-free stabilizers in the form of thicker ones powders, granules or flakes. It facilitates their transport, packing and dosing, and also tremendously improve the wa¬ fire and explosion safety the safety and security of people, hired in their manufacture and use.

The attached examples fully illustrate the method as in invention.

Example I. Up to 0.1 mole of technical melted stearic acid, heated to 100- 105 ° C., 1.18 g of 60% water are added with stirring sorbitol solution and 0.025 mol of brown in portions Cadmium oxide of special purity. Received the mass is heated for 1 hour at the temperature 130-140 ° C - practically to the disappearance of brown oxide cadmium. The thus obtained cadmium stearate is mixed then mixed with 3.6 g of paraffin oil and 0.35 g of oil lycon and squeak if necessary from any small contamination at a temperature of about 120 ° C.

It is introduced into the exaggerated cadmium stearate 0.025 moles of the octahydrate hydroxide in portions barium at temperatures up to approximately 103 ° C. After introducing adding barium hydride and partially "removing it" By taking water, the reacting mass is still warming up 1 hour at 130-140 ° C. Half-way, the molten mass is granulated. 37.92 g is obtained a non-dusty product with properties presented in the table in combination with the stabilized properties of blockages obtained by the known method described on page 1 line 4-9.

Blackboard The stabilizer is produced by according to the invention Stabilizer in production | known method Temperature melting ° C 120-130 135-160 Content bar % 9.1 11 Content cadmium % 7 8.1 Weight heaped g / dm3 55.8 34.9 Heat stabilization hard PVC films 180 ° C 190 ° C min 110 60-70 | <110 60 1 The use of octahydrate sodium hydroxide instead of the water-free one used so far hydroxide or barium oxide facilitates and accelerates the ionic course of the neutralization reaction of stearic acid it or lauric. The addition of one of the above mentioned any fluid released can be carried out reacting the production of stearates and laurates barium-cadmium at temperatures well below higher than used in known methods, viz 130-140 ° C, which effectively prevents darkening and ter-, disintegration of the resulting products and facilitates their granulation or flaking.

The presence of these additives not only makes it easier the course of the reaction is also reduced in stearates and laurates 55 60 Example II. Following example I> with 0.1 mole of stearic acid and 0.025 mole of brown cadmium oxide in the presence of 1.77 g of 60% aqueous sorbitol solution, cadmium stearate is obtained, which, after filtering, is cooled and ground. Until so received our own powdered cadmium stearate was introduced 0.025 mole of octahydrate hydroxide is employed and stirred at room temperature until obtained kite homogeneous mixture. Then after the elapse about 30 minutes, without interrupting mixing, turns on the heat right. At a temperature of 60-70 ° C., 3.6 g are introduced glycerol monostearate and the whole is heated at the same temperature temperature of 130-140 ° C in approximately 1 hour. Received-. The semi-liquid homogeneous mass is subject to flake-195171 no. 37.6 g of a product with the properties are obtained as in example I.

Example III. Cadmium stearate, obtained as in the example Iz 0.1 mole of stearic acid, 0.025 moles of brown cadmium oxide in the presence of 1.18 g of a 60% aqueous sorbitol solution and 3.6 g of a vapor oil fin, cooled and ground. Powdered stearate cadmium is then dosed continuously and evenly with 0.025 mole of octahydrate hydroxide constant dosing at the time of dosing molar ratios - to the heated apparatus, working a continuous system provided with a suitable mix The bench in which the introduced substrates are subjected to reaction while stirring and heating to temperature 130-140 ° C. Proceeding further as in example I, 37.5 g of barium cadmium stearate are obtained with the same good properties as in example I.

Example IV. Up to 0.1 mole of lauric acid heated to 100-105 ° C, it is introduced with stirring 0.92 g of a 60% water solution of sorbitol and porridges 0.025 moles of brown cadmium oxide. Received the mass is heated for 1 hour at the temperature 130-140 ° C, practically until the brown oxide disappears cadmium. Without interrupting mixing, add 2.74 g paraffin oil and 0.14 g of silicone oil and - if needs - suck from possible minor neglect cleaning at a temperature of around 120 ° C. To be sent cadmium laurate is charged in a batch m and 0.025 mole of barium hydroxide octahydrate 6 at temperatures up to approximately 103 ° C. After move in barium hydroxide and after partial removal of water the reaction mass heats up within 1 hour at temperature 130-140 ° C. Semi-liquid molten mass after cooling is subject to grinding. You get 29.1 g a non-dusting product with good stabilizing properties with a melting point of 125-136 ° C water, 2.2% water, 11.2% barium and 9.2% cadmium. io

Claims (4)

Patent claims 1. Process for the production of barium cadmium stearates and laurates by the fusion process, characterized in that brown cadmium oxide is neutralized with an excess of stearic or lauric acid in the presence of a catalyst and the excess of stearic or lauric acid is neutralized with octahydroxy hydroxide. with barium stearate in the environment of the obtained cadmium laurate or stearate, in the presence of a release agent. 2. The method according to claim A method as claimed in claim 1, characterized in that the technical stearic or lauric acid used for the neutralization is used in excess, preferably in molar amounts. 3. The method according to p. A process as claimed in claim 1, characterized in that an aqueous sorbitol solution, preferably 60%, is used as the catalyst. A method according to claim 1, characterized in that paraffin oil, paraffin, ethyl alcohol and glycerol mono stearate are used as the flowable.