CN114292214B - Alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and preparation method thereof - Google Patents
Alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and preparation method thereof Download PDFInfo
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical class N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000010556 emulsion polymerization method Methods 0.000 title description 2
- 239000003085 diluting agent Substances 0.000 claims abstract description 21
- 238000007720 emulsion polymerization reaction Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 125000000129 anionic group Chemical group 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000013543 active substance Substances 0.000 claims description 18
- 238000006386 neutralization reaction Methods 0.000 claims description 18
- 238000004458 analytical method Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 11
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 10
- YBBLOADPFWKNGS-UHFFFAOYSA-N 1,1-dimethylurea Chemical compound CN(C)C(N)=O YBBLOADPFWKNGS-UHFFFAOYSA-N 0.000 claims description 10
- IEORSVTYLWZQJQ-UHFFFAOYSA-N 2-(2-nonylphenoxy)ethanol Chemical compound CCCCCCCCCC1=CC=CC=C1OCCO IEORSVTYLWZQJQ-UHFFFAOYSA-N 0.000 claims description 10
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 10
- 239000001630 malic acid Substances 0.000 claims description 10
- 235000011090 malic acid Nutrition 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229920000847 nonoxynol Polymers 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- 238000004073 vulcanization Methods 0.000 claims description 6
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- -1 nonylphenol ethoxy compound Chemical class 0.000 claims description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims 1
- 239000006172 buffering agent Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 11
- 238000005987 sulfurization reaction Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- TUMNHQRORINJKE-UHFFFAOYSA-N 1,1-diethylurea Chemical compound CCN(CC)C(N)=O TUMNHQRORINJKE-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- MOCKWYUCPREFCZ-UHFFFAOYSA-N chondroitin sulfate E (GalNAc4,6diS-GlcA), precursor 5a Chemical compound NNC(=O)NC1=CC=CC=C1 MOCKWYUCPREFCZ-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000012875 nonionic emulsifier Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method of alkylphenol ethoxylated ammonium sulfate for emulsion polymerization. The alkylphenol ethoxylated ammonium sulfate with low color is prepared by optimizing the production process and adding the buffering agent. Meanwhile, the volatile content of the product is reduced by adding a nonionic diluent, and the mass ratio of the alkylphenol ethoxylate to the nonionic diluent is 100: an optimal level was reached at 28.8. The alkylphenol ethoxylated ammonium sulfate salt is convenient and quick to produce and use and is environment-friendly.
Description
Technical Field
The invention belongs to the technical field of surfactants, and particularly relates to an alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and a preparation method thereof.
Background
The alkylphenol ethoxylated ammonium sulfate is used as a derivative of alkylphenol ethoxy compounds, has nonionic and anionic surface activities due to ethoxy and sulfuric acid groups in molecules, has the excellent characteristics of alkylphenol ethoxy compounds, and has the advantages of stronger foamability, detergency, permeability, emulsifying property, excellent hard water resistance, good calcium soap dispersion phase, remarkable solubilizing capability and small irritation to human bodies. Therefore, the water-based emulsion becomes an important auxiliary agent for cosmetics and various household and industrial products.
At present, the preparation method of alkylphenol ethoxylated ammonium sulfate adopts sulfamic acid and alkylphenol ethoxylate to carry out vulcanization reaction. However, the existing products contain 13-16% of ethanol, and when the products are used for producing water-based polymers, the ethanol solution volatilizes, so that a large amount of volatile components are generated, and the environment is influenced. And the color is high, the paint is pasty at normal temperature, the production of the water-based polymer is not facilitated, and the produced polymer paint film is easy to yellow.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above-mentioned and conventional problems occurring in the prior art.
Accordingly, the present invention is directed to an alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and a process for preparing the same.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided: an alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and a preparation method thereof, comprising,
dehydrating the alkylphenol ethoxylate; mixing the dehydrated alkylphenol ethoxylate, a vulcanizing agent and a vulcanizing catalyst for reaction to obtain a colorless product, adding a nonionic diluent, a buffering agent and deionized water for mixing, adjusting the pH value, and obtaining the alkylphenol ethoxylated ammonium sulfate after the vulcanizing reaction is completed.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the chemical formula of the alkylphenol ethoxylate is shown as follows; wherein R represents the number of carbon atoms and is 5-20; n is the degree of polymerization.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: and the dehydration is carried out by introducing inert gas into alkylphenol ethoxylate for replacement, and heating to 40-60 ℃ until the moisture content is less than 5%.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: such vulcanizing agents include, but are not limited to, sulfamic acid; the vulcanization catalyst is one or more of alkyl or phenyl substituent urea compounds, including but not limited to one or more of N, N-dimethyl urea, N, N-diethyl urea and 4-phenyl semicarbazide.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the mixing reaction may further comprise the step of,
firstly adding the dehydrated alkylphenol ethoxylate and the vulcanization catalyst into a reaction kettle, stirring for 20min, then slowly adding the vulcanization agent, heating to 110-130 ℃, and reacting for 3-5 h.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the mol ratio of the alkylphenol ethoxylate to the vulcanizing agent to the vulcanizing catalyst is 1:1 to 1.2:0.01 to 0.1.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the nonionic diluent comprises one or two of polyethylene glycol and polypropylene glycol with molecular weight of 100-800, and the addition amount is 15-20% of the total mass.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the buffering agent comprises one or more of phosphoric acid, citric acid and malic acid, and the addition amount is 0.01-0.05% of the total mass; the addition amount of the deionized water is 15-20% of the total mass, so that the solid content is 60-62%.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the pH value is adjusted to 9-10 by NaOH or KOH.
As a preferable scheme of the alkylphenol ethoxylated ammonium sulfate for emulsion polymerization and the preparation method thereof, the invention comprises the following steps: the vulcanization reaction is completed, and the content of the anionic active matters of the alkylphenol ethoxylated ammonium sulfate salt of the final product is 58-60%.
The invention has the beneficial effects that:
the invention provides a preparation method of alkylphenol ethoxylated ammonium sulfate for emulsion polymerization. The alkylphenol ethoxylated ammonium sulfate with low color is prepared by optimizing the production process and adding the buffering agent. Meanwhile, the volatile content of the product is reduced by adding a nonionic diluent, and the mass ratio of the nonylphenol ethoxylate to the nonionic diluent is 100: an optimal level was reached at 28.8. The alkylphenol ethoxylated ammonium sulfate salt is convenient and quick to produce and use and is environment-friendly.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The content, chromaticity and viscosity of the anionic active substances detected in the embodiment of the invention are determined according to the following method:
anionic active content determination criteria: GB/T5173-2018 surfactant, detergent and anionic active matter content determination, direct two-phase titration method;
colorimetric determination criteria: GB/T3143-1982 liquid chemical product colour assay;
viscosity measurement standard: GB/T22235-2008 liquid viscosity measurement;
the reagents used in the examples of the present invention are commercially available unless otherwise specified.
Example 1:
100g of nonylphenol ethoxylate (n=4) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.2%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.2g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. 29.2g of sulfamic acid was then slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the sampled and detected anionic active substances reaches more than 94 percent.
38g of pure water, 30g of nonionic diluent PEG-200 g of malic acid, 2g of sodium hydroxide and 10g of sodium hydroxide are added into a neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 10, viscosity 100mpa, s, pH 8.5, active content after 20 minutes stirring: 60.5%.
Example 2:
100g of nonylphenol ethoxylate (n=10) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 1%, and the oxygen content is less than 0.2%.
After the water content is qualified, 2.28g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. Then 16.9g of sulfamic acid was slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the sampled and detected anionic active substances reaches more than 94 percent.
38g of pure water, 28.8g of nonionic diluent PPG-200, 2g of malic acid and 15g of sodium hydroxide are added into the neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 100, viscosity 151mpa, s, pH 7.65, active content after 20 minutes stirring: 59.8%.
Example 3:
100g of nonylphenol ethoxylate (n=10) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.5%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.28g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. Then 16.9g of sulfamic acid was slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the anionic active substances is detected by sampling.
38g of pure water, 28.8g of nonionic diluent PPG-200, 2g of malic acid and 15g of sodium hydroxide are added into the neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 45, viscosity 151mpa, s, pH 7.65, active content after 20 minutes stirring: 60.2%.
Example 4:
100g of nonylphenol ethoxylate (n=10) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.2%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.28g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. Then 16.9g of sulfamic acid was slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the anionic active substances is detected by sampling.
38g of pure water, 28.8g of nonionic diluent PPG-200, 2g of malic acid and 15g of sodium hydroxide are added into the neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 10, viscosity 151mpa, s, pH 7.65, active content after 20 minutes stirring: 59.9%.
Example 5:
100g of nonylphenol ethoxylate (n=4) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.2%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.2g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. 29.2g of sulfamic acid was then slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the anionic active substances is detected by sampling.
38g of pure water, 28.8g of nonionic diluent PEG-200, 2g of malic acid and 10g of sodium hydroxide are added into a neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 10, viscosity 100mpa, s, pH 8.5, active content after 20 minutes stirring: 60.2%.
Example 6:
100g of nonylphenol ethoxylate (n=4) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.2%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.2g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. 29.2g of sulfamic acid was then slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the anionic active substances is detected by sampling.
38g of pure water, 200 g of nonionic diluent PEG-200 g of malic acid, 2g of sodium hydroxide and 10g of sodium hydroxide are added into a neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 10, viscosity 100mpa, s, pH 8.5, active content after 20 minutes stirring: 60.5%.
Example 7:
100g of nonylphenol ethoxylate (n=4) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.2%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.2g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. 29.2g of sulfamic acid was then slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the anionic active substances is detected by sampling.
38g of pure water, 200 g of nonionic diluent PEG-40 g of malic acid, 2g of sodium hydroxide and 10g of sodium hydroxide are added into a neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 10, viscosity 100mpa, s, pH 8.5, active content after 20 minutes stirring: 52.2%.
Example 7:
100g of nonylphenol ethoxylate (n=4) is added into a normal pressure reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to 60 ℃, water is sampled and analyzed, the water content is required to be less than 0.2%, and the oxygen content is required to be less than 0.2%.
After the water content is qualified, 2.2g of sulfuration catalyst N, N-dimethyl urea is added and stirred for 10 minutes. 29.2g of sulfamic acid was then slowly added and stirred for 10 minutes. The reaction kettle is heated to 130 ℃ and reacts for 1 hour, and the content of the anionic active substances is detected by sampling.
38g of pure water, 200 g of nonionic diluent PEG-40 g of malic acid, 2g of sodium hydroxide and 10g of sodium hydroxide are added into a neutralization kettle and stirred for 20 minutes. The sample analysis pH was 10. And after the content of the anionic active substances in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle. Sample analysis color 10, viscosity 100mpa, s, pH 8.5, active content after 20 minutes stirring: 52.2%.
Example 8:
the volatile content was determined for each of examples 1 to 7 and the commercially available samples, as follows:
test methods gas chromatography was performed according to ISO 11890-2 color paint and varnish Volatile Organic Compound (VOC) content determination. Sample 1 was purchased from Shanghai loyalty fine chemical, CO-436, and sample 2 was purchased from Sorvy, CO-436.
The comparative data obtained are as follows:
TABLE 1
The addition of a nonionic diluent can reduce the viscosity of the product because the alkylphenol ethoxylates are compatible with the nonionic diluent, because the nonionic diluent has a boiling point in excess of 260 ℃ and only small amounts of volatile organics are produced when detecting VOCs. However, when the non-ionic diluent is added in an amount exceeding 20% by mass, the product performance is adversely affected, and when the non-ionic emulsifier is added in an amount exceeding 20% by mass, the final product active content is less than 58%, which affects the downstream application of the product.
Example 9:
the procedure of example 1 was repeated except that the alkylphenol ethoxylate was replaced with the starting alkylphenol. And detecting the obtained product. The specific cases are shown in Table 2.
TABLE 2
The invention provides a preparation method of alkylphenol ethoxylated ammonium sulfate for emulsion polymerization. The alkylphenol ethoxylated ammonium sulfate with low color is prepared by optimizing the production process and adding the buffering agent. Meanwhile, the volatile content of the product is reduced by adding a nonionic diluent, and the mass ratio of the alkylphenol ethoxylate to the nonionic diluent is 100: an optimal level was reached at 28.8. The alkylphenol ethoxylated ammonium sulfate salt is convenient and quick to produce and use and is environment-friendly.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (1)
1. A preparation method of alkylphenol ethoxylated ammonium sulfate for emulsion polymerization is characterized in that: comprising the steps of (a) a step of,
adding 100g of nonylphenol ethoxylate into a normal pressure reaction kettle, introducing nitrogen into the reaction kettle, heating to 60 ℃, sampling and analyzing water, wherein the water content is required to be less than 0.2%, and the oxygen content is less than 0.2%;
after the moisture is qualified, adding 2.2g of vulcanization catalyst N, N-dimethylurea, stirring for 10 minutes, then slowly adding 29.2g of sulfamic acid, stirring for 10 minutes, heating the reaction kettle to 130 ℃, reacting for 1 hour, sampling and detecting the content of anionic active substances;
38g of pure water, 200 g of nonionic diluent PEG-200 g of malic acid, 2g of sodium hydroxide and 10g of sodium hydroxide are added into a neutralization kettle, stirred for 20 minutes, and the pH value of the sample analysis is 10; after the content of the anionic active matters in the reaction kettle is more than 90%, transferring the materials in the reaction kettle into a neutralization kettle, stirring for 20 minutes, sampling and analyzing the materials with chromaticity of 10, viscosity of 100mpa, s and pH of 8.5, wherein the content of the active matters is as follows: 60.5%;
the chemical formula of the nonylphenol ethoxy compound is shown as the specification, wherein R is C 9 H 19 ，n＝4。
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