Preparation method of blocky solid defoaming agent

Abstract

The invention relates to a preparation method of a blocky solid defoaming agent, which comprises the following steps: premixing a defoaming active matter and an emulsifier, stirring and mixing with paraffin at a certain temperature, and cooling and molding the mixed material to obtain the blocky solid defoaming agent. Wherein the emulsifier can ensure that the defoaming active matter can be uniformly dissolved and dispersed in a foaming system, so that an excellent defoaming effect is achieved. Paraffin is relatively high in hydrophobicity, so that not only can the performance of the product be enhanced, but also the blocky product can be ensured to realize a long-term foam eliminating and inhibiting function in flowing foaming liquid.

Description

Technical Field

[0001] The invention relates to a method for preparing a block solid defoamer. The defoamer belongs to fine chemical preparations, so the invention belongs to the technical field of fine chemical preparations. Background Art

[0002] Defoaming agents are now widely used in food, petrochemical, textile, printing and dyeing, papermaking, medicine, fermentation, chemical and other fields due to their ability to destroy and inhibit foam.

[0003] Defoamers can be divided into liquid defoamers and solid defoamers according to their form. Liquid defoamers generally have disadvantages such as poor stability, stratification after long-term storage, and high transportation costs. Solid defoamers have attracted much attention from researchers since their advent due to their simple process, good storage stability, good defoaming and suppression properties, and low transportation costs.

[0004] Patents US2004116316A1 and WO95026691A1 prepare powdered solid defoamers by spraying active materials, adhesives and water-soluble carriers. The prepared defoamers have uniform density and are close to the density of powdered laundry detergents prepared by spray granulation. Therefore, the defoamers can be well dispersed therein and will not separate after long-term storage.

[0005] Patent CN102085428B premixes a composite emulsifier, polyether-modified silicone, glycerol polyether and glycerol ester, and then mixes them with a composite inorganic salt, and then dries, crushes and sieves them to obtain a powdered solid defoamer, which has excellent defoaming and defoaming performance at high temperatures.

[0006] Patents CN101991976B and CN102302869B first premix the defoaming active substance, emulsifier, and structurant, then add the organic carrier and deionized water into the mixer in sequence and stir evenly, then granulate the mixture through a granulator and dry it in a dryer to obtain a granular solid defoamer. The solid defoamer prepared by the method has a denser structure and therefore has excellent flow properties and anti-attenuation properties.

[0007] On the whole, the solid defoamer prepared by the patent is mostly in powder or granular form. Although it can be mixed in powder and used as an internal addition, it is still not ideal in the flowing foaming liquid, such as sewage treatment and metal processing, and the ability to suppress foam is not well controlled. Patent CN103550961B has developed a block solid defoamer that can be adapted to use in flowing foaming liquid and convenient to put in or take out of the foaming liquid at will. It first neutralizes the fatty acid mixed in proportion with sodium hydroxide solution to generate fatty acid salt, and then compound it with active ingredients, emulsifiers, and structural agents. After mixing evenly, acid-base regulators are appropriately added, and the material is discharged and packed in plastic bags after cooling, and further cooled and formed to obtain solid block products. This process is simple and feasible, but the fatty acid salt has good solubility, which causes it to be consumed too quickly in aqueous solution, and it is difficult to achieve a long-term defoaming function. At the same time, fatty acid salts also have a certain foaming ability, which may affect the defoaming performance of the final product. Summary of the invention

[0008] The present invention relates to a method for preparing a block solid defoamer, wherein a defoaming active substance is pre-mixed with an emulsifier, and then stirred and mixed with paraffin at a certain temperature, and the mixed material is cooled and formed to obtain a block solid defoamer. The emulsifier can ensure that the defoaming active substance can be uniformly dissolved and dispersed in the foaming system, thereby achieving an excellent defoaming and depressing effect. Paraffin wax has strong hydrophobicity, which can not only enhance the performance of the product, but also ensure that the block product can achieve a long-term defoaming and depressing function in the flowing foaming liquid.

[0009] The blocky solid defoamer of the present invention comprises the following components: A. Antifoaming active ingredients The defoaming active substance is prepared by the known technology in the technical field, mainly made of polyorganosiloxane, catalyst, silicone resin and silicon dioxide; the amount used accounts for 5-40% of the total mass of the solid defoaming agent; B. Emulsifier The emulsifier is a nonionic surfactant, specifically a mixture of polyether and polyether-modified polysiloxane; the amount of polyether accounts for 10-40% of the total mass of the emulsifier; the amount of the emulsifier accounts for 5-20% of the total mass of the solid defoamer; The polyether structural formula is: R[O(EO) a (PO) b H] m . Wherein R is a straight or branched alkyl group with 3 to 30 carbon atoms, a and b are the degree of polymerization, specifically integers of 10 to 60, and m is the functionality, specifically 1 to 3; The structural formula of polyether modified polysiloxane is as follows: (CH 3 ) 3 SiO[(CH3 ) 2 SiO] p [CH 3 QSiO] q Si(CH 3 ) 3 , where Q = -R4O(EO) r (PO) s R5, p=0-50, q=0-50, r=0-20, s=0-30, R4 is hydrogen, an alkyl group having 2-3 carbon atoms; R5 is hydrogen, an alkyl group having 1-3 carbon atoms; C. Structuring agent The structural agent is paraffin, the melting point is 40-80°C, and the amount used accounts for 50-85% of the total mass of the defoamer; The preparation method of the block solid defoamer comprises the following specific steps: (1) Add the defoaming active ingredient A and the emulsifier B into the mixer M1 and stir evenly; (2) Add paraffin wax into mixer M2 and heat it to 60-100°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 60-100°C and the stirring time is 0.5-2.0h. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0010] Specific implementation methods

[0011] Antifoam Active Examples

[0012] Prepared by referring to the technical solution of Example 1 of Patent ZL201410325381.0

[0013] Polyether Examples

[0014]

[0015] Polyether modified polysiloxane embodiment

[0016]

[0017] Example of block solid defoamer

[0018] Example 1

[0019] (1) Add 5 g of defoaming active ingredient, 1.5 g of polyether 1, and 13.5 g of polyether-modified polysiloxane 1 into a mixer M1 and stir evenly; (2) Add 80 g of paraffin wax with a melting point of 42°C into the mixer M2 and heat it to 60°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. Keep the temperature at 60°C and stir for 2 hours. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0020] Example 2 (1) Add 15 g of defoaming active ingredient, 2 g of polyether 2, and 8 g of polyether-modified polysiloxane 2 into a mixer M1 and stir evenly; (2) Add 75 g of paraffin wax with a melting point of 56°C into the mixer M2 and heat it to 70°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. Keep the temperature at 70°C and stir for 1 hour. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0021] Example 3 (1) Add 30 g of defoaming active material, 2 g of polyether 3, and 3 g of polyether-modified polysiloxane 3 into a mixer M1 and stir evenly; (2) Add 65 g of paraffin wax with a melting point of 65°C into the mixer M2 and heat it to 80°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 80°C and the stirring time is 1.5 h. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0022] Example 4 (1) Add 20 g of defoaming active material, 6 g of polyether 4, and 14 g of polyether-modified polysiloxane 4 into a mixer M1 and stir evenly; (2) Add 60 g of paraffin wax with a melting point of 73°C into the mixer M2 and heat it to 90°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 90°C and the stirring time is 2 hours. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0023] Example 5 (1) Add 7 g of defoaming active ingredient, 3 g of polyether 5, and 5 g of polyether-modified polysiloxane 5 into a mixer M1 and stir evenly; (2) Add 85 g of paraffin wax with a melting point of 80°C into the mixer M2 and heat it to 100°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 100°C and the stirring time is 1 hour. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0024] Example 6 (1) Add 40 g of defoaming active ingredient, 2.5 g of polyether 6, and 7.5 g of polyether-modified polysiloxane 6 into a mixer M1 and stir evenly; (2) Add 50 g of paraffin wax with a melting point of 75°C into the mixer M2 and heat it to 90°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 90°C and the stirring time is 0.5 h. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0025] Comparative Example 1 (1) Add 5 g of defoaming active ingredient and 15 g of polyether-modified polysiloxane 1 into a mixer M1 and stir evenly; (2) Add 80 g of paraffin wax with a melting point of 42°C into the mixer M2 and heat it to 60°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. Keep the temperature at 60°C and stir for 2 hours. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0026] Comparative Example 2 (1) Add 15 g of defoaming active ingredient and 10 g of polyether 2 into mixer M1 and stir evenly; (2) Add 75 g of paraffin wax with a melting point of 56°C into the mixer M2 and heat it to 70°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. Keep the temperature at 70°C and stir for 1 hour. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

[0027] Comparative Example 3 (1) Add 30 g of defoaming active material, 2 g of polyether 3, and 3 g of polyether-modified polysiloxane 3 into a mixer M1 and stir evenly; (2) Add 65 g of polyacrylate with a molecular weight of 5000 into mixer M2 and heat it to 80° C. to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 80°C and the stirring time is 1.5 h. (4) The mixture obtained in (3) is dried, cooled and formed to obtain the prepared block solid defoaming agent.

[0028] Anti-foaming performance test Washing machine test Test method: Add 50g of commercially available laundry detergent and 0.3g of solid defoamer to a drum washing machine with a capacity of 7kg, and the test procedure is standard washing. There are 11 measurement marks on the door of the washing machine, which are recorded as 0, 10, 20...100, where 0 is the start, indicating no foam; 100 indicates full of foam. Every 5 minutes is a washing cycle, and the foam height is recorded every 5 minutes, and the data is recorded when the machine is stopped. The larger the value, the higher the foam height in the washing machine, and the worse the foam suppression effect; the lower the foam height in the same time, the better the product's foam suppression performance. The test results are as follows: Washing Machine Test Results

[0029] Note: In the above table, "X" means the test at that time; "Y" means the sample was tested after being placed at a temperature of 40°C and a humidity of 70% for four weeks.

[0030] Through the above tests, it can be seen that the block solid defoamer sample prepared by this method has good defoaming and antifoaming performance both in the early and late stages of washing; and after being placed at a temperature of 40°C and a humidity of 70% for four weeks, the defoaming and antifoaming performance does not change significantly, and has good stability.

Claims

1. A method for preparing a block solid defoamer, characterized in that: The preparation method is as follows: (1) Add the defoaming active ingredient A and the emulsifier B into the mixer M1 and stir evenly; (2) Add paraffin wax into mixer M2 and heat it to 60-100°C to melt it; (3) After the paraffin is completely melted into liquid, add the mixture in (1) into the mixer M2 and stir evenly. The insulation temperature is 60-100°C and the stirring time is 0.5-2.0h. (4) The mixture obtained in (3) is cooled and formed to obtain the prepared block solid defoaming agent.

2. The method for preparing a block solid defoamer according to claim 1, characterized in that: The defoaming active substance A is prepared by the known technology in the technical field, and is mainly prepared from polyorganosiloxane, catalyst, silicone resin and silicon dioxide; the amount used accounts for 5-40% of the total mass of the solid defoaming agent.

3. The method for preparing a block solid defoamer according to claim 1, characterized in that: The emulsifier is a nonionic surfactant, specifically a mixture of polyether and polyether-modified polysiloxane; the amount of polyether accounts for 10-40% of the total mass of the emulsifier; the amount of the emulsifier accounts for 5-20% of the total mass of the solid defoamer.

4. The method for preparing a block solid defoamer according to claim 3, characterized in that: The polyether structural formula is: R[O(EO) a (PO) b H] m Wherein R is a straight or branched alkyl group having 3 to 30 carbon atoms, a and b are the degree of polymerization, specifically integers of 10 to 60, and m is the functionality, specifically an integer of 1 to 3.

5. The method for preparing a block solid defoamer according to claim 3, characterized in that: The structural formula of the polyether-modified polysiloxane is: (CH3)3SiO[(CH3)2SiO] p [CH3QSiO] q Si(CH3)3, where Q = -R4O(EO) r (PO) s R5, p=0-50, q=0-50, r=0-20, s=0-30, R4 is hydrogen or an alkyl group having 2-3 carbon atoms; R5 is hydrogen or an alkyl group having 1-3 carbon atoms.

6. The method for preparing a block solid defoamer according to claim 1, characterized in that: The structural agent is paraffin, the melting point of which is between 40 and 80° C., and the amount of the structural agent accounts for 50 to 85% of the total mass of the defoaming agent.

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