CN107541128B - Environment-friendly waterproof emulsion and preparation method thereof - Google Patents
Environment-friendly waterproof emulsion and preparation method thereof Download PDFInfo
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- CN107541128B CN107541128B CN201610481999.5A CN201610481999A CN107541128B CN 107541128 B CN107541128 B CN 107541128B CN 201610481999 A CN201610481999 A CN 201610481999A CN 107541128 B CN107541128 B CN 107541128B
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Abstract
The invention discloses an environment-friendly waterproof emulsion which comprises the following components in parts by weight: 89-93 parts of an emulsifier DSB; 130-34 parts of emulsifier COPS-130; 4740 parts of butyl acrylate and 4760 parts of acrylic acid; 1700 portions of styrene and 1740 portions; 128 portions of acrylamide and 136 portions; 33-37 parts of sodium persulfate; 18-22 parts of tert-butyl hydroperoxide; 10-20 parts of a reducing agent; 10-50 parts of a pH regulator; 60-90 parts of post-additive; water 5000-. The used materials do not contain harmful substances such as formaldehyde, APEO, NPEO and the like, and the VOC content of the materials is extremely low.
Description
Technical Field
The invention relates to the field of waterproof coatings, in particular to an environment-friendly waterproof emulsion and a preparation method thereof.
Background
The waterproof emulsion on the market at present has various varieties and uneven quality, and in the preparation of the traditional waterproof emulsion, the used materials mostly contain toxic and harmful substances such as formaldehyde, alkylphenol polyoxyethylene ether compounds (APEO) or Nonylphenol Polyoxyethylene Ether (NPEO) and the like, and the substances not only have great harm to the health of human bodies, but also have the influence on the ecological environment in the aspects of toxicity, poor biodegradability, environmental hormone generation, harmful byproducts generation in the production process and the like; or the waterproof emulsion contains Volatile Organic Compounds (VOC) which has great influence on human health, when the VOC in a room reaches a certain concentration, people can feel headache, nausea, vomiting, hypodynamia and the like in a short time, and can be convulsion and coma in severe cases, and the liver, kidney, brain and nervous system of people can be injured, so that serious consequences such as hypomnesis and the like can be caused.
Therefore, developing a waterproof emulsion which is prepared from materials without using toxic and harmful substances and does not generate volatile organic compounds is a crucial topic in the waterproof emulsion industry at present.
Disclosure of Invention
The invention aims to provide an environment-friendly waterproof emulsion which is made of materials which do not contain harmful substances such as formaldehyde, APEO (alkylphenol ethoxylates), NPEO and the like and have extremely low VOC (volatile organic compounds) content.
In order to achieve the purpose, the invention provides the following technical scheme:
an environment-friendly waterproof emulsion comprises the following components in parts by weight:
the reducing agent is at least one of vitamin E and vitamin C.
Wherein, disodium alkyl diphenyl oxide Disulfonate (DSB) and sodium allyloxy hydroxypropyl sulfonate (COPS-1) are used as emulsifiers, and both are anionic reactive emulsifiers. DSB as an anionic polysulfonate surfactant has two anionic groups, can provide the attractive force between outstanding molecules, enables the molecules to be easy to interact with other molecules containing single ions or large organic matters, can improve the mechanical stability and the temperature stability of latex, and can effectively reduce the dosage of the surfactant; the COPS-1 molecular structure contains hydroxyl and sulfonic group and is polymerized with styrene, so that the solubility of latex can be obviously improved, and the raw material does not contain APEO and NPEO and simultaneously provides good chemical properties; the tert-butyl hydroperoxide is used as an initiator of polymerization reaction, and is eliminated after monomers are polymerized without residue, so that the content of VOC in the waterproof emulsion is greatly reduced. Preferably, the reducing agent is vitamin E, the vitamin E is a fat-soluble vitamin and replaces conventional sodium formaldehyde sulfoxylate as the reducing agent, the vitamin E is less than a water-soluble vitamin such as vitamin C in material consumption and high in efficiency, and the reducing performance is provided on the premise that the raw material does not contain formaldehyde.
Preferably, the post-additive comprises the following components in parts by weight: 9-11 parts of a defoaming agent; 33-37 parts of a dispersing agent; 9-11 parts of a bactericide; 9-31 parts of thickening agent, wherein the defoaming agent is a metal stearate compound, the dispersing agent is sodium polyacrylate, the bactericide is dibromonitrilopropionamide, the thickening agent is associative acrylic acid, and the raw materials do not contain formaldehyde, APEO, NPEO and other harmful substances, so that the aim of preparing the environment-friendly waterproof emulsion is fulfilled.
The preparation method of the environment-friendly waterproof emulsion comprises the following steps:
step 1: adding water, an emulsifier DSB, an emulsifier COPS-1, butyl acrylate, styrene and acrylamide into an emulsifying tank in sequence, and stirring to form stable emulsion;
step 2: adding a proper amount of water into a reaction kettle, stirring and heating to 86 ℃;
and step 3: adding the sodium persulfate aqueous solution I into a reaction kettle;
and 4, step 4: dropwise adding a sodium persulfate aqueous solution II and the emulsion obtained in the step 1 into the reaction kettle at the temperature of 86-88 ℃;
the specific operation is as follows:
p1: dropwise adding the emulsion obtained in the step 1 for 3.4-4 hours;
p2: dropwise adding a second aqueous sodium persulfate solution 2 hours after the start of the dropwise adding process in P1, and dropwise adding a second aqueous sodium persulfate solution 5 minutes after the end of the dropwise adding process in P1;
and 5: preserving the temperature of the mixture obtained in the step 4 at 88 ℃ for 60-70 minutes, and then cooling to 70 ℃;
step 6: performing post-treatment on the mixture obtained in the step 5, dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a reducing agent aqueous solution, and preserving heat at 70 ℃;
the specific operation is as follows:
s1: performing one-time post-treatment on the mixture obtained in the step 5, dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a reducing agent aqueous solution for 1 hour, and preserving heat for 30-35 minutes after dropwise adding;
s2: performing secondary post-treatment on the mixture obtained in the step S1, dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a reducing agent aqueous solution for 1 hour, and preserving heat for 30-35 minutes after dropwise adding;
and 7: cooling the mixture obtained in the step 6 and simultaneously performing air draft treatment;
and 8: when the temperature is reduced to 50 ℃ in the step 7, adding a PH regulator, and adjusting the PH value to 7-8;
and step 9: when the temperature is reduced to 45 ℃ in the step 7, adding a defoaming agent, a dispersing agent, a bactericide, a thickening agent and water;
step 10: when the temperature is reduced to 40 ℃ in step 7, the mixture is taken out and filtered and packaged by a 60-mesh filter bag.
Further preferably in the present invention, the aqueous tert-butyl hydroperoxide solution comprises the following components in parts by weight: 9-11 parts of tert-butyl hydroperoxide and 75 parts of water; the reducing agent aqueous solution comprises the following components in parts by weight: 5-10 parts of a reducing agent and 75 parts of water.
In the preparation process, carrying out post-treatment twice in the step 6, carrying out heat preservation after the primary post-treatment is finished, carrying out secondary post-treatment, giving a certain heat preservation time while prolonging the post-treatment time to continue the reaction of the residual monomers, fully eliminating the residual monomers generated in the reaction process in the repeated post-treatment twice, and generating a very small amount of toxic volatile substances in the post-treatment process, thereby greatly reducing the content of VOC in the waterproof emulsion; in step 7, the mixture is subjected to an air draft treatment while being cooled, and residual monomers in the mixture are extracted, so that the VOC content in the emulsion reaches a very low level.
Preferably, the pressure in the emulsification tank in the step 1 is 0.05-0.15MPa, and the raw materials in the emulsification tank react under a certain pressure, so that the reaction in the emulsification tank can be more sufficient, the amount of residual monomers is reduced, and the content of VOC in the waterproof emulsion is further reduced.
Preferably, in the P1, the dropping flow rate within 10 minutes after the start of dropping is 0.6 times the average flow rate, and the dropping flow rate within 20 minutes before the end of dropping is 0.8 times the average flow rate; the flow of the sodium persulfate aqueous solution II in the P2 is uniform in the whole process. The first sodium persulfate aqueous solution comprises the following components in parts by weight: 25-27 parts of sodium persulfate and 100 parts of water; the second sodium persulfate aqueous solution comprises the following components in parts by weight: 8-10 parts of sodium persulfate and 150 parts of water. Adopting relatively slow dropping acceleration at the initial stage of dropping the emulsion to enable the emulsion to slowly react with the initial initiator sodium persulfate aqueous solution, increasing the flow after the reaction is carried out for a period of time, preventing a large amount of residual monomers from being generated by sudden reaction, and reducing the flow when the dropping process is about to end so that the emulsion which is not reacted at the early stage can fully react before the dropping process is ended, and preventing residual unreacted residual monomers from being remained; the flow of the second sodium persulfate aqueous solution is uniform in the whole process, the dropwise addition of the second sodium persulfate aqueous solution is finished 5 minutes after the end of the dropwise addition process in the P1, and the slow flow before the end of the dropwise addition is matched, so that the emulsion and the initiator are fully reacted before the end of the dropwise addition process, the amount of residual monomers is reduced, and the content of VOC in the waterproof emulsion is reduced.
The invention has the advantages that:
1. disodium alkyl diphenyl ether Disulfonate (DSB) and sodium allyloxy hydroxypropyl sulfonate (COPS-1) are used as emulsifying agents, vitamin E and vitamin C are used as reducing agents, and the used materials do not contain harmful substances such as formaldehyde, APEO and NPEO;
2. the raw materials in the emulsifying tank react under certain pressure, so that the reaction is more sufficient, the amount of residual monomers is reduced, and the content of VOC in the waterproof emulsion is reduced;
3. residual monomers generated in the reaction process are fully eliminated in the repeated post-treatment for two times, and a very small amount of toxic volatile substances are generated in the post-treatment process, so that the content of VOC in the waterproof emulsion is greatly reduced;
4. and (3) performing air draft treatment while cooling the mixture, and pumping out residual monomers in the mixture, so that the VOC content in the emulsion reaches a very low level.
Drawings
FIG. 1 is a flow chart of the preparation process of the environment-friendly waterproof emulsion of the present invention.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that the preparation methods described in the examples are only for illustrating the present invention and are not to be construed as limiting the present invention, and that the simple modifications of the preparation methods of the present invention based on the concept of the present invention are within the scope of the present invention as claimed.
All materials referred to in the examples of the present invention are commercially available.
The first embodiment is as follows:
(1) 1525kg of water, 91kg of emulsifier DSB, 32kg of emulsifier COPS-1, 4750kg of butyl acrylate, 1720kg of styrene and 357kg of acrylamide aqueous solution are sequentially added into an emulsification tank and stirred for 30 minutes, wherein the acrylamide aqueous solution comprises 225kg of water and 132kg of acrylamide, and the pressure in the emulsification tank is 0.1MPa, so that a stable emulsion is formed;
(2) adding 2200kg of water into a reaction kettle, stirring and heating to 86 ℃;
(3) adding a first sodium persulfate aqueous solution into a reaction kettle, wherein the first sodium persulfate aqueous solution comprises 100kg of water and 26kg of sodium persulfate;
(4) dropwise adding the emulsion obtained in the step (1) into a reaction kettle, wherein the dropwise adding time is 3.5-4 hours, the average flow is 37kg/min, the dropwise adding temperature is 86-88 ℃, the dropwise adding flow within 10 minutes after the dropwise adding is started is 22.2kg/min, and the dropwise adding flow within 20 minutes before the dropwise adding is finished is 29.6 kg/min;
(5) beginning to uniformly drop a second sodium persulfate aqueous solution 2 hours after the beginning of the dropping process in the step (4), and ending dropping the second sodium persulfate aqueous solution 5 minutes after the end of the dropping process in the step (4), wherein the second sodium persulfate aqueous solution comprises 150kg of water and 9kg of sodium persulfate;
(6) preserving the temperature of the mixture obtained in the step (5) at 88 ℃ for 60 minutes, and then cooling to 70 ℃;
(7) performing one-time post-treatment on the mixture obtained in the step (6), dropwise adding a tert-butyl hydroperoxide aqueous solution and a vitamin E aqueous solution, wherein the dropwise adding time is 1 hour, and the temperature is kept for 30 minutes after the dropwise adding is finished, the tert-butyl hydroperoxide aqueous solution comprises 75kg of water and 10kg of tert-butyl hydroperoxide, and the vitamin E aqueous solution comprises 75kg of water and 6kg of vitamin E;
(8) performing secondary post-treatment on the mixture obtained in the step (7), dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a vitamin E aqueous solution for 1 hour, and preserving heat for 30 minutes after dropwise adding;
(9) cooling the mixture obtained in the step (8) and simultaneously performing air draft treatment;
(10) when the temperature in the step (9) is reduced to 50 ℃, 125kg of water is added, and caustic soda flakes are added to serve as a pH regulator, so that the pH value is adjusted to 7-8;
(11) when the temperature in the step (9) is reduced to 45 ℃, 10kg of metal stearate compound is added to serve as a defoaming agent, 35kg of polyacrylic acid sodium salt serves as a dispersing agent, 10kg of dibromo nitrilo propionamide serves as a bactericide, 15kg of associated acrylic acid serves as a thickening agent, and 650kg of water;
(12) when the temperature in (9) is reduced to 40 ℃, taking out the mixture and filtering and packaging the mixture by using a 60-mesh filter bag, thereby obtaining the environment-friendly waterproof emulsion.
Example two:
(1) 1530kg of water, 93kg of emulsifier DSB, 34kg of emulsifier COPS-1, 4760kg of butyl acrylate, 1700kg of styrene and 357kg of acrylamide aqueous solution are sequentially added into an emulsification tank and stirred for 30 minutes, wherein the acrylamide aqueous solution comprises 221kg of water and 136kg of acrylamide, and the pressure in the emulsification tank is 0.05MPa, so that a stable emulsion is formed;
(2) adding 2250kg of water into a reaction kettle, stirring and heating to 86 ℃;
(3) adding a first sodium persulfate aqueous solution into a reaction kettle, wherein the first sodium persulfate aqueous solution comprises 100kg of water and 25kg of sodium persulfate;
(4) dropwise adding the emulsion obtained in the step (1) into a reaction kettle, wherein the dropwise adding time is 3.5-4 hours, the average flow is 36kg/min, the dropwise adding temperature is 86-88 ℃, the dropwise adding flow within 10 minutes after the dropwise adding is started is 21.6kg/min, and the dropwise adding flow within 20 minutes before the dropwise adding is finished is 28.8 kg/min;
(5) beginning to uniformly drop a second sodium persulfate aqueous solution 2 hours after the beginning of the dropping process in the step (4), and ending dropping the second sodium persulfate aqueous solution 5 minutes after the end of the dropping process in the step (4), wherein the second sodium persulfate aqueous solution comprises 150kg of water and 10kg of sodium persulfate;
(6) preserving the temperature of the mixture obtained in the step (5) at 88 ℃ for 60 minutes, and then cooling to 70 ℃;
(7) performing one-time post-treatment on the mixture obtained in the step (6), dropwise adding a tert-butyl hydroperoxide aqueous solution and a vitamin E aqueous solution, wherein the dropwise adding time is 1 hour, and the temperature is kept for 35 minutes after the dropwise adding is finished, the tert-butyl hydroperoxide aqueous solution comprises 75kg of water and 9kg of tert-butyl hydroperoxide, and the vitamin E aqueous solution comprises 75kg of water and 7kg of vitamin E;
(8) performing secondary post-treatment on the mixture obtained in the step (7), dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a vitamin E aqueous solution for 1 hour, and preserving heat for 35 minutes after dropwise adding is finished;
(9) cooling the mixture obtained in the step (8) and simultaneously performing air draft treatment;
(10) when the temperature in the step (9) is reduced to 50 ℃, 125kg of water is added, and caustic soda flakes are added to serve as a pH regulator, so that the pH value is adjusted to 7-8;
(11) when the temperature in the step (9) is reduced to 45 ℃, 10kg of metal stearate compound is added to serve as a defoaming agent, 35kg of polyacrylic acid sodium salt serves as a dispersing agent, 10kg of dibromo nitrilo propionamide serves as a bactericide, 15kg of associated acrylic acid serves as a thickening agent, and 650kg of water;
(12) when the temperature in (9) is reduced to 40 ℃, taking out the mixture and filtering and packaging the mixture by using a 60-mesh filter bag, thereby obtaining the environment-friendly waterproof emulsion.
Example three:
(1) 1520kg of water, 89kg of emulsifier DSB, 30kg of emulsifier COPS-1, 4740kg of butyl acrylate, 1740kg of styrene and 357kg of acrylamide aqueous solution are sequentially added into an emulsifying tank and stirred for 30 minutes, wherein the acrylamide aqueous solution comprises 229kg of water and 128kg of acrylamide, and the pressure in the emulsifying tank is 0.15MPa, so that a stable emulsion is formed;
(2) adding 2200kg of water into a reaction kettle, stirring and heating to 86 ℃;
(3) adding a first sodium persulfate aqueous solution into a reaction kettle, wherein the first sodium persulfate aqueous solution comprises 100kg of water and 27kg of sodium persulfate;
(4) dropwise adding the emulsion obtained in the step (1) into a reaction kettle, wherein the dropwise adding time is 3.5-4 hours, the average flow is 38kg/min, the dropwise adding temperature is 86-88 ℃, the dropwise adding flow within 10 minutes after the dropwise adding is started is 22.8kg/min, and the dropwise adding flow within 20 minutes before the dropwise adding is finished is 30.4 kg/min;
(5) beginning to uniformly drop a second sodium persulfate aqueous solution 2 hours after the beginning of the dropping process in the step (4), and ending dropping the second sodium persulfate aqueous solution 5 minutes after the end of the dropping process in the step (4), wherein the second sodium persulfate aqueous solution comprises 150kg of water and 8kg of sodium persulfate;
(6) preserving the temperature of the mixture obtained in the step (5) at 88 ℃ for 60 minutes, and then cooling to 70 ℃;
(7) performing one-time post-treatment on the mixture obtained in the step (6), dropwise adding a tert-butyl hydroperoxide aqueous solution and a vitamin E aqueous solution, wherein the dropwise adding time is 1 hour, and the temperature is kept for 30 minutes after the dropwise adding is finished, the tert-butyl hydroperoxide aqueous solution comprises 75kg of water and 11kg of tert-butyl hydroperoxide, and the vitamin E aqueous solution comprises 75kg of water and 5kg of vitamin E;
(8) performing secondary post-treatment on the mixture obtained in the step (7), dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a vitamin E aqueous solution for 1 hour, and preserving heat for 30 minutes after dropwise adding;
(9) cooling the mixture obtained in the step (8) and simultaneously performing air draft treatment;
(10) when the temperature in the step (9) is reduced to 50 ℃, 125kg of water is added, ammonia water is added to be used as a pH regulator, and the pH value is adjusted to 7-8;
(11) when the temperature in the step (9) is reduced to 45 ℃, 10kg of metal stearate compound is added to serve as a defoaming agent, 35kg of polyacrylic acid sodium salt serves as a dispersing agent, 10kg of dibromo nitrilo propionamide serves as a bactericide, 15kg of associated acrylic acid serves as a thickening agent, and 650kg of water;
(12) when the temperature in (9) is reduced to 40 ℃, taking out the mixture and filtering and packaging the mixture by using a 60-mesh filter bag, thereby obtaining the environment-friendly waterproof emulsion.
Comparative example one:
at present, chinese patent with application publication No. CN104693943A discloses a preparation method of a waterproof emulsion, and the examples thereof are as follows:
preparation of polymer emulsion: taking 100 parts of deionized water by weight, adding the deionized water into a reaction kettle, and then sequentially adding 2 parts of sodium octadecyl sulfonate and an emulsifier TX-13: 2 parts of pH value regulator, 2 parts of pentadiene, 6 parts of acrylic acid, 10 parts of methyl methacrylate, 10 parts of n-butyl methacrylate, 5 parts of glutaric acid and 1 part of ammonium persulfate, heating to 60 ℃ at the speed of 5 ℃/min, fully stirring for 10 hours, wherein the stirring speed is 400 r/min, heating to 75 ℃ at the speed of 3 ℃/min, continuing to fully stir for 5 hours, wherein the stirring speed is 400 r/min, then adding 3 parts of EDTA, degassing under the vacuum condition, then adjusting the pH value to 7 by using a NaOH solution with the mass percentage of 20%, cooling to the room temperature at the speed of 3 ℃/min, and obtaining a polymer emulsion;
preparation of the coating: taking 1 part of dispersing agent, 1 part of defoaming agent, 1 part of flatting agent, 20 parts of nano titanium dioxide and 20 parts of silicon dioxide microspheres by weight, adding the dispersing agent, 40 parts of polymer emulsion by weight, stirring and dispersing at a stirring speed of 400 rpm, then adding 1.5 parts of bentonite and 5 parts of filler, continuing stirring for 2 hours at a stirring speed of 400 rpm, grinding for 2 hours, and filtering by using a paint filter to obtain the waterproof paint.
Comparative example two:
different from the first embodiment, in the step (7) and the step (8), sodium formaldehyde sulfoxylate (rongalite) is used as a reducing agent instead of vitamin E, and the aqueous solution of sodium formaldehyde sulfoxylate comprises 75kg of water and 20kg of sodium formaldehyde sulfoxylate.
Comparative example three:
different from the first embodiment, in the step (1), the emulsification tank has no certain internal pressure when the reaction is carried out.
Comparative example four:
the difference from the first embodiment is that after the post-treatment is finished, the air draft treatment is not performed in the step (9).
Comparative example five:
the difference from the first example is that the second aftertreatment in step (8) is not carried out.
The first and second comparative examples differ from the examples in that:
the first comparative example mainly adopts an emulsifier TX-13, and as TX-13 is alkylphenol ethoxylates, the used material contains harmful substances such as APEO, NPEO and the like; in the second comparative example, the commonly used rongalite is used as a reducing agent instead of vitamin E, and obviously, the raw materials contain formaldehyde.
Compared with the environment-friendly waterproof emulsion produced in the first to third embodiments of the invention, the results of various performance tests are shown in Table 1.
Table 1 examples and comparative examples each obtained performance test results
As can be seen from comparison of Table 1, compared with the prior art, the environment-friendly waterproof emulsion produced by the invention does not contain harmful substances such as formaldehyde, APEO, NPEO and the like, and the content of VOC in the waterproof emulsion is extremely low, so that the environment-friendly waterproof emulsion is superior to the existing waterproof emulsion in environmental protection performance.
Claims (3)
1. A preparation method of environment-friendly waterproof emulsion is characterized by comprising the following steps:
(1) 1525kg of water, 91kg of emulsifier DSB, 32kg of emulsifier COPS-1, 4750kg of butyl acrylate, 1720kg of styrene and 357kg of acrylamide aqueous solution are sequentially added into an emulsification tank and stirred for 30 minutes, wherein the acrylamide aqueous solution comprises 225kg of water and 132kg of acrylamide, and the pressure in the emulsification tank is 0.1MPa, so that a stable emulsion is formed;
(2) adding 2200kg of water into a reaction kettle, stirring and heating to 86 ℃;
(3) adding a first sodium persulfate aqueous solution into a reaction kettle, wherein the first sodium persulfate aqueous solution comprises 100kg of water and 26kg of sodium persulfate;
(4) dropwise adding the emulsion obtained in the step (1) into a reaction kettle, wherein the dropwise adding time is 3.5-4 hours, the average flow is 37kg/min, the dropwise adding temperature is 86-88 ℃, the dropwise adding flow within 10 minutes after the dropwise adding is started is 22.2kg/min, and the dropwise adding flow within 20 minutes before the dropwise adding is finished is 29.6 kg/min;
(5) beginning to uniformly drop a second sodium persulfate aqueous solution 2 hours after the beginning of the dropping process in the step (4), and ending dropping the second sodium persulfate aqueous solution 5 minutes after the end of the dropping process in the step (4), wherein the second sodium persulfate aqueous solution comprises 150kg of water and 9kg of sodium persulfate;
(6) preserving the temperature of the mixture obtained in the step (5) at 88 ℃ for 60 minutes, and then cooling to 70 ℃;
(7) performing one-time post-treatment on the mixture obtained in the step (6), dropwise adding a tert-butyl hydroperoxide aqueous solution and a vitamin E aqueous solution, wherein the dropwise adding time is 1 hour, and the temperature is kept for 30 minutes after the dropwise adding is finished, the tert-butyl hydroperoxide aqueous solution comprises 75kg of water and 10kg of tert-butyl hydroperoxide, and the vitamin E aqueous solution comprises 75kg of water and 6kg of vitamin E;
(8) performing secondary post-treatment on the mixture obtained in the step (7), dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a vitamin E aqueous solution for 1 hour, and preserving heat for 30 minutes after dropwise adding;
(9) cooling the mixture obtained in the step (8) and simultaneously performing air draft treatment;
(10) when the temperature in the step (9) is reduced to 50 ℃, 125kg of water is added, and caustic soda flakes are added to serve as a pH regulator, so that the pH value is adjusted to 7-8;
(11) when the temperature in the step (9) is reduced to 45 ℃, 10kg of metal stearate compound is added to serve as a defoaming agent, 35kg of polyacrylic acid sodium salt serves as a dispersing agent, 10kg of dibromo nitrilo propionamide serves as a bactericide, 15kg of associated acrylic acid serves as a thickening agent, and 650kg of water;
(12) when the temperature in (9) is reduced to 40 ℃, taking out the mixture and filtering and packaging the mixture by using a 60-mesh filter bag, thereby obtaining the environment-friendly waterproof emulsion.
2. A preparation method of environment-friendly waterproof emulsion is characterized by comprising the following steps: (1) 1530kg of water, 93kg of emulsifier DSB, 34kg of emulsifier COPS-1, 4760kg of butyl acrylate, 1700kg of styrene and 357kg of acrylamide aqueous solution are sequentially added into an emulsification tank and stirred for 30 minutes, wherein the acrylamide aqueous solution comprises 221kg of water and 136kg of acrylamide, and the pressure in the emulsification tank is 0.05MPa, so that a stable emulsion is formed;
(2) adding 2250kg of water into a reaction kettle, stirring and heating to 86 ℃;
(3) adding a first sodium persulfate aqueous solution into a reaction kettle, wherein the first sodium persulfate aqueous solution comprises 100kg of water and 25kg of sodium persulfate;
(4) dropwise adding the emulsion obtained in the step (1) into a reaction kettle, wherein the dropwise adding time is 3.5-4 hours, the average flow is 36kg/min, the dropwise adding temperature is 86-88 ℃, the dropwise adding flow within 10 minutes after the dropwise adding is started is 21.6kg/min, and the dropwise adding flow within 20 minutes before the dropwise adding is finished is 28.8 kg/min;
(5) beginning to uniformly drop a second sodium persulfate aqueous solution 2 hours after the beginning of the dropping process in the step (4), and ending dropping the second sodium persulfate aqueous solution 5 minutes after the end of the dropping process in the step (4), wherein the second sodium persulfate aqueous solution comprises 150kg of water and 10kg of sodium persulfate;
(6) preserving the temperature of the mixture obtained in the step (5) at 88 ℃ for 60 minutes, and then cooling to 70 ℃;
(7) performing one-time post-treatment on the mixture obtained in the step (6), dropwise adding a tert-butyl hydroperoxide aqueous solution and a vitamin E aqueous solution, wherein the dropwise adding time is 1 hour, and the temperature is kept for 35 minutes after the dropwise adding is finished, the tert-butyl hydroperoxide aqueous solution comprises 75kg of water and 9kg of tert-butyl hydroperoxide, and the vitamin E aqueous solution comprises 75kg of water and 7kg of vitamin E;
(8) performing secondary post-treatment on the mixture obtained in the step (7), dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a vitamin E aqueous solution for 1 hour, and preserving heat for 35 minutes after dropwise adding is finished;
(9) cooling the mixture obtained in the step (8) and simultaneously performing air draft treatment;
(10) when the temperature in the step (9) is reduced to 50 ℃, 125kg of water is added, and caustic soda flakes are added to serve as a pH regulator, so that the pH value is adjusted to 7-8;
(11) when the temperature in the step (9) is reduced to 45 ℃, 10kg of metal stearate compound is added to serve as a defoaming agent, 35kg of polyacrylic acid sodium salt serves as a dispersing agent, 10kg of dibromo nitrilo propionamide serves as a bactericide, 15kg of associated acrylic acid serves as a thickening agent, and 650kg of water;
(12) when the temperature in the step (9) is reduced to 40 ℃, taking out the mixture and filtering and packaging the mixture by using a 60-mesh filter bag, thereby obtaining the environment-friendly waterproof emulsion.
3. A preparation method of environment-friendly waterproof emulsion is characterized by comprising the following steps: (1) 1520kg of water, 89kg of emulsifier DSB, 30kg of emulsifier COPS-1, 4740kg of butyl acrylate, 1740kg of styrene and 357kg of acrylamide aqueous solution are sequentially added into an emulsifying tank and stirred for 30 minutes, wherein the acrylamide aqueous solution comprises 229kg of water and 128kg of acrylamide, and the pressure in the emulsifying tank is 0.15MPa, so that a stable emulsion is formed;
(2) adding 2200kg of water into a reaction kettle, stirring and heating to 86 ℃;
(3) adding a first sodium persulfate aqueous solution into a reaction kettle, wherein the first sodium persulfate aqueous solution comprises 100kg of water and 27kg of sodium persulfate;
(4) dropwise adding the emulsion obtained in the step (1) into a reaction kettle, wherein the dropwise adding time is 3.5-4 hours, the average flow is 38kg/min, the dropwise adding temperature is 86-88 ℃, the dropwise adding flow within 10 minutes after the dropwise adding is started is 22.8kg/min, and the dropwise adding flow within 20 minutes before the dropwise adding is finished is 30.4 kg/min;
(5) beginning to uniformly drop a second sodium persulfate aqueous solution 2 hours after the beginning of the dropping process in the step (4), and ending dropping the second sodium persulfate aqueous solution 5 minutes after the end of the dropping process in the step (4), wherein the second sodium persulfate aqueous solution comprises 150kg of water and 8kg of sodium persulfate;
(6) preserving the temperature of the mixture obtained in the step (5) at 88 ℃ for 60 minutes, and then cooling to 70 ℃;
(7) performing one-time post-treatment on the mixture obtained in the step (6), dropwise adding a tert-butyl hydroperoxide aqueous solution and a vitamin E aqueous solution, wherein the dropwise adding time is 1 hour, and the temperature is kept for 30 minutes after the dropwise adding is finished, the tert-butyl hydroperoxide aqueous solution comprises 75kg of water and 11kg of tert-butyl hydroperoxide, and the vitamin E aqueous solution comprises 75kg of water and 5kg of vitamin E;
(8) performing secondary post-treatment on the mixture obtained in the step (7), dropwise adding a tert-butyl hydrogen peroxide aqueous solution and a vitamin E aqueous solution for 1 hour, and preserving heat for 30 minutes after dropwise adding;
(9) cooling the mixture obtained in the step (8) and simultaneously performing air draft treatment;
(10) when the temperature in the step (9) is reduced to 50 ℃, 125kg of water is added, ammonia water is added to be used as a pH regulator, and the pH value is adjusted to 7-8;
(11) when the temperature in the step (9) is reduced to 45 ℃, 10kg of metal stearate compound is added to serve as a defoaming agent, 35kg of polyacrylic acid sodium salt serves as a dispersing agent, 10kg of dibromo nitrilo propionamide serves as a bactericide, 15kg of associated acrylic acid serves as a thickening agent, and 650kg of water;
(12) when the temperature in (9) is reduced to 40 ℃, taking out the mixture and filtering and packaging the mixture by using a 60-mesh filter bag, thereby obtaining the environment-friendly waterproof emulsion.
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| CN101386663A (en) * | 2008-10-30 | 2009-03-18 | 上海三瑞高分子材料有限公司 | Multifunctional acrylic ester emulsion |
| CN102492081A (en) * | 2011-11-29 | 2012-06-13 | 广东达美新材料有限公司 | Preparation method of self-crosslinking microemulsion with high solid content |
| CN104271263A (en) * | 2012-03-29 | 2015-01-07 | 威士伯采购公司 | Waterborne underbody coating system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101386663A (en) * | 2008-10-30 | 2009-03-18 | 上海三瑞高分子材料有限公司 | Multifunctional acrylic ester emulsion |
| CN102492081A (en) * | 2011-11-29 | 2012-06-13 | 广东达美新材料有限公司 | Preparation method of self-crosslinking microemulsion with high solid content |
| CN104271263A (en) * | 2012-03-29 | 2015-01-07 | 威士伯采购公司 | Waterborne underbody coating system |
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