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CN112011006A - High-absorptivity resin for removing adult urine odor and preparation method thereof - Google Patents

High-absorptivity resin for removing adult urine odor and preparation method thereof Download PDF

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Publication number
CN112011006A
CN112011006A CN202010735339.1A CN202010735339A CN112011006A CN 112011006 A CN112011006 A CN 112011006A CN 202010735339 A CN202010735339 A CN 202010735339A CN 112011006 A CN112011006 A CN 112011006A
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odor
deodorant
adult urine
absorbent resin
extract
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CN112011006B (en
Inventor
杨卫东
刘健
吕志平
刘新
阮玉林
韩伟恒
朱雅亮
邵东
裴小苏
刘若铎
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Zhejiang Satellite Science & Technology Co ltd
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Zhejiang Satellite Science & Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/346—Clay
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/19—Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Dispersion Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Absorbent Articles And Supports Therefor (AREA)

Abstract

The invention discloses a high-absorptivity resin for removing adult urine odor and a preparation method thereof. A method for preparing a super absorbent resin for removing adult urine odor, comprising the steps of: a. acrylic acid, deionized water, a water-soluble initiator, a bridging agent, a dispersing agent and an adsorbing material containing a deodorant are polymerized in a reactor containing a stirring device to generate colloid; b. the colloid formed in step a is crushed, granulated and neutralized with an alkaline substance, including but not limited to sodium hydroxide; c. and drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin for removing the odor of adult urine. The high-absorptivity resin for removing the odor of the adult urine and the preparation method thereof disclosed by the invention have the advantages of simple production process and excellent product absorption performance, and particularly can effectively remove the odor of the adult urine.

Description

High-absorptivity resin for removing adult urine odor and preparation method thereof
Technical Field
The invention belongs to the field of fine chemical engineering, and particularly relates to a preparation method of high-absorptivity resin for removing adult urine odor and high-absorptivity resin for removing adult urine odor.
Background
Super Absorbent Polymer (SAP) is a functional Polymer material that is insoluble in water and organic solvents. The molecular chain of the polymer contains hydrophilic groups such as carboxyl, amido, sulfonic group and the like, is a strong hydrophilic polymer with a macromolecular cross-linked three-dimensional network structure, and has a high water absorption function of absorbing several hundred to thousands times of the weight of the polymer. In addition, the SAP, which is highly swollen after absorbing water, has excellent water retention ability, and the formed gel has good strength and is not easy to squeeze out water even when pressurized.
The high-absorptivity resin has already been produced industrially in a mature way, and is mainly applied to the field of disposable sanitary materials, such as baby diapers, adult diapers, sanitary napkins, nursing pads and the like. The SAP for adult paper diapers and nursing pads mainly has the performance requirements of large absorption capacity, good dryness, bacteriostasis, deodorization and the like at present, and has prominent functional requirements on bacteriostasis and deodorization, particularly on eliminating the smell of urine along with the continuous improvement of the life quality of people. Patent CN104403249 describes a method for preparing super absorbent resin by using nano silver antibacterial agent, nano silver has certain effect on bacteriostasis, but basically has no deodorizing function. Patent CN102428110 combines SAP with chelating agent and tannin to improve deodorization, but the deodorization effect only has effect on released ammonia gas, and the effect on adult urine is not obvious. Patent CN202337750 covers the aromatic substance with beta-cyclodextrin, which can slow down the release speed to the outside, and the beta-cyclodextrin can be slowly released after the water absorption resin absorbs the liquid, so as to achieve the effect of deodorization. However, the release of the aromatic substances only covers the odor, and the actual deodorization effect cannot be achieved.
Disclosure of Invention
The present invention is directed to the state of the art, overcomes the above drawbacks, and provides a method for preparing a super absorbent resin for removing adult urine odor and a super absorbent resin for removing adult urine odor.
The invention discloses a high-absorptivity resin for removing adult urine odor and a preparation method thereof, and mainly aims to add an adsorbing material containing a deodorant in a polymerization process, release a part of the deodorant to eliminate odor while adsorbing a part of odor, add a plant-type deodorant in a surface treatment process to further neutralize the odor, and further improve the environmental odor by the special fragrance of plants.
The invention adopts the following technical scheme that the preparation method of the high-absorptivity resin for removing the adult urine odor comprises the following steps:
a. acrylic acid, deionized water, a water-soluble initiator, a bridging agent, a dispersing agent and an adsorbing material containing a deodorant are polymerized in a reactor containing a stirring device to generate colloid;
b. the colloid formed in step a is crushed, granulated and neutralized with an alkaline substance, including but not limited to sodium hydroxide;
c. drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin for removing the odor of adult urine;
d. and c, treating the semi-finished product in the step c at a preset surface treatment temperature under the action of a surface cross-linking agent and a plant deodorant to obtain a finished product of the high-absorptivity resin for removing the adult urine smell.
According to the technical scheme, as a further preferable technical scheme of the technical scheme, the adsorbing material containing the deodorant is prepared by mixing the deodorant and the inorganic adsorbing material at a high speed, the mixing rotating speed is 2000-5000rpm, and the using amount of the adsorbing material containing the deodorant is 0.1-10% of acrylic acid.
According to the technical scheme, as a further preferable technical scheme of the technical scheme, the deodorant is one or more selected from the group consisting of octyl trimethyl ammonium chloride, decyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, octyl pyridine chloride, dodecyl pyridine chloride, tetradecyl pyridine chloride, methyl tridecyl ammonium bromide, methyl tridecyl ammonium chloride, methyl tridecyl ammonium bromide, methyl triacontyl ammonium chloride and methyl triacontyl ammonium bromide, and the dosage of the deodorant is 0.01% -25% of the adsorbent containing the deodorant.
According to the technical scheme, as a further preferable technical scheme of the technical scheme, the inorganic adsorption material is selected from one or more of activated carbon, molecular sieve, zeolite, kaolin, silica sol, nano-silica, nano-carbon dioxide and clay, and the dosage of the inorganic adsorption material is 75-99.9% of that of the adsorption material containing the deodorant.
According to the technical scheme, as a further preferable technical scheme of the technical scheme, the bridging agent is one or more selected from pentaerythritol tetraacrylic acid, N' -methylene bisacrylamide, polyethylene glycol diacrylate, pentaerythritol triallyl ether, pentaerythritol triacrylate and triallylamine ester, and the dosage of the bridging agent is 0.05-5% of the mass of acrylic acid.
According to the above technical means, as a further preferable technical means of the above technical means, the dispersant is one or more selected from sucrose fatty acid ester, octadecyl phosphate, monoglyceride, sorbitan monooleate, sorbitan tristearate, ethylene glycol distearate, a castor oil/hydrogenated castor oil and ethylene oxide condensate, triglycerol monostearate, propylene glycol monostearate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, and carboxymethyl cellulose, and the amount of the dispersant is 0.001 to 1% by mass of acrylic acid.
According to the above technical means, as a further preferable technical means of the above technical means, the surface cross-linking agent is one or more selected from ethanol, ethylene glycol, diethylene glycol, polyethylene glycol, glycerol, polyglycerol, isopropanol, 1, 4-butanediol, diethanolamine, triethanolamine, polyoxypropylene ether, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, and glycerol diglycidyl ether, and the amount of the surface cross-linking agent is 1% to 10% of the semi-finished product of the high-absorbency resin for removing the odor of adult urine.
According to the above technical means, as a further preferable technical means of the above technical means, the plant type deodorant is one or more selected from the group consisting of thyme extract, sophora flavescens extract, cinnamon extract, senecio italica extract, mustard extract, horseradish extract, chitin extract and cardamom extract, and the amount of the plant type deodorant is 0.01-10% of the semi-finished product of the high-absorptivity resin for removing the urine odor of an adult.
According to the above technical means, as a further preferable technical means of the above technical means, the preset surface treatment temperature in the step d is 60 to 200 ℃.
The invention also discloses a high-absorptivity resin for removing the adult urine odor, which is prepared by the preparation method of the high-absorptivity resin for removing the adult urine odor disclosed by any one technical scheme.
The high-absorptivity resin for removing the odor of adult urine and the preparation method thereof have the advantages of simple production process and excellent product absorption performance, and particularly can effectively remove the odor of adult urine.
Detailed Description
The invention discloses a preparation method of a high-absorptivity resin for removing adult urine odor and a high-absorptivity resin for removing adult urine odor, and the specific implementation mode of the invention is further described by combining a preferred embodiment.
Preferred embodiments.
Preferably, the method for preparing the super absorbent resin for removing the odor of the adult urine comprises the following steps:
a. acrylic acid, deionized water, a water-soluble initiator, a bridging agent, a dispersing agent and an adsorbing material containing a deodorant are polymerized in a reactor containing a stirring device to generate colloid;
b. the colloid formed in step a is crushed, granulated and neutralized with an alkaline substance, including but not limited to sodium hydroxide;
c. drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin for removing the odor of adult urine;
d. and c, treating the semi-finished product in the step c at a preset surface treatment temperature under the action of a surface cross-linking agent and a plant deodorant to obtain a finished product of the high-absorptivity resin for removing the adult urine smell.
Further, the adsorbent containing the deodorant is prepared by mixing the deodorant and the inorganic adsorbent at a high speed of 2000-5000rpm, and the amount of the adsorbent containing the deodorant is 0.1-10% of that of acrylic acid.
Further, the deodorant is selected from one or more of octyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, octyl pyridine chloride, decyl pyridine chloride, dodecyl pyridine chloride, tetradecyl pyridine chloride, methyl tridecyl ammonium bromide, methyl tridecyl ammonium chloride, methyl tridecyl ammonium bromide, methyl triacontyl ammonium chloride and methyl triacontyl ammonium bromide, and the dosage of the deodorant is 0.01% -25% of the adsorbing material containing the deodorant.
Further, the inorganic adsorption material is selected from one or more of activated carbon, molecular sieve, zeolite, kaolin, silica sol, nano-silica, nano-carbon dioxide and clay, and the dosage of the inorganic adsorption material is 75-99.9% of that of the adsorption material containing the deodorant.
Furthermore, the bridging agent is selected from one or more of pentaerythritol tetraacrylic acid, N' -methylene bisacrylamide, polyethylene glycol diacrylate, pentaerythritol triallyl ether, pentaerythritol triacrylate and triallylamine ester, and the dosage of the bridging agent is 0.05-5% of the mass of the acrylic acid.
Further, the dispersing agent is selected from one or more of sucrose fatty acid ester, octadecyl phosphate, monoglyceride, sorbitan monooleate, sorbitan tristearate, ethylene glycol distearate, a castor oil/hydrogenated castor oil and ethylene oxide condensate, triglycerol monostearate, propylene glycol monostearate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose and carboxymethyl cellulose, and the using amount of the dispersing agent is 0.001-1% of the mass of acrylic acid.
Further, the surface cross-linking agent is selected from one or more of ethanol, ethylene glycol, diethylene glycol, polyethylene glycol, glycerol, polyglycerol, isopropanol, 1, 4-butanediol, diethanolamine, triethanolamine, polyoxypropylene ether, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether and glycerol diglycidyl ether, and the dosage of the surface cross-linking agent is 1% -10% of the semi-finished product of the high-absorptivity resin for removing the odor of adult urine.
Further, the plant deodorant is selected from one or more of thyme extract, sophora flavescens extract, cinnamon extract, Helichrysum italicum extract, mustard extract, horseradish extract, chitin extract and cardamom extract, and the amount of the plant deodorant is 0.01-10% of the semi-finished product of the high-absorptivity resin for removing the urine odor of adults.
Further, the preset surface treatment temperature in the step d is 60-200 ℃.
The embodiment also discloses a high-absorptivity resin for removing the odor of adult urine, which is prepared by the preparation method of the high-absorptivity resin for removing the odor of adult urine, disclosed by any one of the technical schemes in the embodiment.
A first variant embodiment.
Preferably, the method for preparing the super absorbent resin for removing the odor of the adult urine comprises the following steps:
a. acrylic acid, deionized water, a water-soluble initiator, a bridging agent, a dispersing agent and an adsorbing material containing a deodorant are polymerized in a reactor containing a stirring device to generate colloid.
b. Crushing and granulating the colloid formed in the step a, and neutralizing the colloid by using sodium hydroxide or other alkaline substances;
c. drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin;
d. and c, treating the semi-finished product in the step c at a certain temperature under the action of a surface cross-linking agent and a plant deodorant to obtain a high-absorptivity resin finished product.
Purified acrylic acid is used as the acrylic acid, and the monomer concentration of the aqueous acrylic acid solution in step a is 15 to 50%, preferably 20 to 35%, particularly preferably 22 to 32%. The monomer concentration of the acrylic acid aqueous solution is lower than 15 percent, the polymerization is difficult to initiate, the monomer concentration of the acrylic acid aqueous solution is higher than 50 percent, the polymerization reaction is difficult to control, and the implosion reaction is easy to occur.
The water-soluble initiator is an oxidant/reductant initiating system. Wherein the oxidant is selected from one or more of sodium persulfate, potassium persulfate, ammonium persulfate and hydrogen peroxide; the reducing agent is selected from one or more of sodium bisulfite, ferrous sulfate and ascorbic acid. The mass ratio of the oxidant to the reducing agent is (0.5-2): (0.5 to 2), preferably 1: (1-2). The dosage of the oxidant is 0.002-0.08 percent of the mass of the acrylic acid.
The bridging agent is selected from one or more of pentaerythritol tetraacrylic acid, N' -methylene bisacrylamide, polyethylene glycol diacrylate, pentaerythritol triallyl ether, pentaerythritol triacrylate and triallylamine ester, and the dosage of the bridging agent is 0.05-5 percent of the mass of acrylic acid, and is preferably 0.1-2 percent. The bridging agent is less than 0.05 percent, the internal crosslinking density of the high-absorptivity resin product is low, the gel strength is poor, and the high-absorptivity resin product is not suitable for being used on sanitary products; the bridging agent is higher than 5 percent, the internal crosslinking density of the high-absorptivity resin product is too high, the water absorption performance of the high-absorptivity resin product is obviously reduced, and the high-absorptivity resin product is not suitable for being used on sanitary articles;
the dispersant is used for uniformly dispersing the absorbent material containing the deodorant in the acrylic monomer solution, and is selected from one or more of sucrose fatty acid ester, octadecyl phosphate, monoglyceride, sorbitan monooleate, sorbitan tristearate, ethylene glycol distearate, castor oil/hydrogenated castor oil and ethylene oxide condensate, triglycerol monostearate, propylene glycol monostearate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose and carboxymethyl cellulose, and the amount of the dispersant is 0.001-1%, preferably 0.01-0.5% of the acrylic acid.
The adsorbing material containing the deodorant is prepared by mixing the deodorant and the inorganic adsorbing material at a high speed, wherein the mixing speed is 2000-5000rpm, and the using amount of the adsorbing material is 0.1-10% relative to the acrylic acid.
The deodorant in the adsorbing material containing the deodorant is selected from one or more of octyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, octyl pyridine chloride, dodecyl pyridine chloride, methyl tridecyl ammonium bromide, methyl tridecyl ammonium chloride, methyl tridecyl ammonium bromide, methyl triacontyl ammonium chloride and methyl triacontyl ammonium bromide, and the dosage of the deodorant is 0.01-25 percent, preferably 0.05-20 percent of the adsorbing material containing the deodorant.
The inorganic adsorption material in the adsorption material containing the deodorant is one or more selected from activated carbon, molecular sieve, zeolite, kaolin, silica sol, nano-silica, nano-carbon dioxide and clay, and the dosage of the inorganic adsorption material is 75-99.9%, preferably 80-99.95% of the adsorption material containing the deodorant.
The adsorbing material containing the deodorant is prepared by mixing the deodorant and the inorganic adsorbing material at a high speed of 2000-5000rpm, so that the deodorant and the inorganic adsorbing material can be uniformly mixed by the high-speed mixing, and the deodorant is adsorbed in the inorganic material, wherein the dosage of the deodorant is 0.1-10%, preferably 0.5-5% relative to the acrylic acid.
The polymerization temperature of the acrylic monomer solution is 0 to 60 ℃ and preferably 0 to 30 ℃. The polymerization time is 20-90 minutes. After the polymerization reaches the highest temperature, the colloid is placed at the temperature of 50-120 ℃ and is kept for 0.5-10 hours.
The gel colloid formed by polymerization is crushed, granulated and neutralized by sodium hydroxide or other alkaline substances.
The auxiliary agent for neutralization during granulation is one or more selected from sodium/potassium hydroxide, sodium/potassium bicarbonate and sodium/potassium carbonate, and the addition form is solid particles or an aqueous solution form thereof. The amount added is 40 to 95%, preferably 60 to 85%, and more preferably 70 to 85% of the molar amount of acrylic acid.
And drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin.
And c, treating the semi-finished product in the step c at a certain temperature under the action of a surface cross-linking agent and a plant deodorant to obtain a high-absorptivity resin finished product.
The surface cross-linking agent is selected from one or more of ethanol, ethylene glycol, diethylene glycol, polyethylene glycol, glycerol, polyglycerol, isopropanol, 1, 4-butanediol, diethanolamine, triethanolamine, polyoxypropylene ether, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether and glycerol diglycidyl ether, and the dosage of the surface cross-linking agent is 1-10% of the semi-finished product of the high-absorptivity resin, preferably 1.5-8%.
The plant deodorant is one or more selected from herba Thymi extract, radix Sophorae Flavescentis extract, cortex Cinnamomi extract, Helichrysum italicum extract, mustard extract, horseradish extract, chitin extract, and fructus Amomi rotundus extract, and is used in an amount of 0.01-10%, preferably 0.1-5% of the high-absorptivity resin semi-finished product. The plant deodorant can further neutralize the smell in urine, and simultaneously, the plant deodorant has faint scent and can improve the smell of the environment.
The surface treatment temperature is 60-200 deg.C, preferably 100-200 deg.C, and the surface treatment time is 20-120 min, preferably 30-90 min.
The embodiment also discloses a high-absorptivity resin for removing the odor of adult urine, which is prepared by the preparation method of the high-absorptivity resin for removing the odor of adult urine, disclosed by any one of the technical schemes in the embodiment.
A second variant embodiment.
Preferably, the method for preparing the super absorbent resin for removing the odor of the adult urine comprises the following steps:
a. acrylic acid, deionized water, a water-soluble initiator, a bridging agent, a dispersing agent and an adsorbing material containing a deodorant are polymerized in a reactor containing a stirring device to generate colloid;
b. crushing and granulating the colloid formed in the step a, and neutralizing the colloid by using sodium hydroxide or other alkaline substances;
c. drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin;
d. and c, treating the semi-finished product in the step c at a certain temperature under the action of a surface cross-linking agent and a plant deodorant to obtain a high-absorptivity resin finished product.
The high-absorptivity resin is prepared by mixing deodorant and inorganic absorbent at high speed, wherein the mixing speed is 2000-5000rpm, and the dosage is 0.1-10% relative to acrylic acid.
The adsorbing material contains deodorant, wherein the deodorant is selected from one or more of octyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, octyl pyridine chloride, dodecyl pyridine chloride, methyl tridecyl ammonium bromide, methyl tridecyl ammonium chloride, methyl tridecyl ammonium bromide, methyl thirty-eight alkyl ammonium chloride and methyl thirty-eight alkyl ammonium bromide, and the dosage of the deodorant is 0.01% -25% of that of the adsorbing material containing the deodorant.
The deodorant-containing adsorbing material is one or more of activated carbon, molecular sieve, zeolite, kaolin, silica sol, nano-silica, nano-carbon dioxide and clay, and the dosage of the deodorant-containing adsorbing material is 75-99.9% of that of the deodorant-containing adsorbing material.
The high-absorptivity resin comprises a bridging agent which is one or more of pentaerythritol tetraacrylic acid, N' -methylene bisacrylamide, polyethylene glycol diacrylate, pentaerythritol triallyl ether, pentaerythritol triacrylate and triallylamine ester, and the dosage of the bridging agent is 0.05-5% of the mass of acrylic acid.
The high-absorptivity resin comprises a dispersant selected from one or more of sucrose fatty acid ester, octadecyl phosphate, monoglyceride, sorbitan monooleate, sorbitan tristearate, ethylene glycol distearate, a condensate of castor oil/hydrogenated castor oil and ethylene oxide, triglycerol monostearate propylene glycol monostearate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose and carboxymethyl cellulose, wherein the amount of the dispersant is 0.001-1% of that of acrylic acid.
The super absorbent resin is characterized in that the surface cross-linking agent is one or more selected from ethanol, ethylene glycol, diethylene glycol, polyethylene glycol, glycerol, polyglycerol, isopropanol, 1, 4-butanediol, diethanolamine, triethanolamine, polyoxypropylene ether, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether and glycerol diglycidyl ether, and the dosage of the super absorbent resin is 1-10% of that of a semi-finished product of the super absorbent resin.
The super absorbent resin and the plant deodorant are selected from one or more of thyme extract, radix Sophorae Flavescentis extract, cortex Cinnamomi extract, Helichrysum italicum extract, mustard extract, horseradish extract, chitin extract, and fructus Amomi rotundus extract, and the dosage is 0.01-10% of the semi-finished product of the super absorbent resin.
The temperature of the surface treatment of the super absorbent resin is 60-200 ℃.
The embodiment also discloses a high-absorptivity resin for removing the odor of adult urine, which is prepared by the preparation method of the high-absorptivity resin for removing the odor of adult urine, disclosed by any one of the technical schemes in the embodiment.
The product performance test method of the specific examples and the comparative examples is as follows:
(1) evaluation method for removing adult urine odor.
A250 mL Erlenmeyer flask was filled with 1.5g SAP and 100g adult urine, sealed with a stopper, placed in a 37 ℃ water bath, and after 2 hours, the cover of the Erlenmeyer flask was opened to smell immediately, and the lower the score, the better the deodorizing effect of the urine.
Watch 1
Odor grade Score value
Has no odor 1
Slight smell 2
Has odor and no irritation 3
Has pungent odor 4
Strong pungent smell 5
Intolerable pungent odor 6
(2) Saline water absorption rate.
The saline absorption Capacity (Free Swelling Capacity) refers to the Free Swelling Capacity of a superabsorbent resin per unit mass in saline over a certain period of time.
Specifically, 0.2000g of super absorbent resin was weighed in a tea bag, immersed in a 0.9 wt% aqueous sodium chloride solution for 30min to allow free expansion, and then suspended for 10min to remove water, thereby obtaining a water absorption capacity (unit; g/g).
Saline absorption rate ═ mAfter absorbing water-mSample (A)-mBlank space)/mSample (A)。
(3) Centrifugal water retention.
The centrifugal Retention Capacity (Centrifuge Retention Capacity) is a water absorption Capacity obtained by freely swelling a high-absorbent resin per unit mass in saline water for a certain period of time and then removing water by a Centrifuge.
Specifically, 0.2000g of super absorbent resin was weighed in a tea bag, immersed in a 0.9 wt% aqueous sodium chloride solution for 30min to be freely swollen, and then dehydrated by a centrifuge (centrifugal force: 250g) to obtain a water absorption capacity (unit; g/g).
Centrifuge retention rate ═ mAfter centrifugation-mSample (A)-mBlank space)/mSample (A)。
(4) Absorption under pressure.
The Absorption Under Pressure (Absorption Under Pressure) refers to the water Absorption rate of a high-absorbent resin per unit mass Under a certain Pressure for a certain time.
Specifically, the water absorption capacity (unit: g/g) was obtained by swelling 0.9000g of a super absorbent resin in a 0.9 wt% aqueous sodium chloride solution for 1 hour under a load of 0.7 psi.
Absorption rate under pressure (m)After absorbing water-mBefore water absorption)/mSample (A)。
(5) The absorption speed.
The Absorption Speed (Absorption Speed) refers to how fast a mass of superabsorbent resin absorbs saline.
Specifically, 50mL of 0.9 wt% sodium chloride aqueous solution is added into a 100mL beaker, 2.0000g of high-absorptivity resin is added into the beaker under magnetic stirring (rotating speed of 600r/min), timing is started, the timing is stopped after the liquid level vortex disappears to the recovery level, and the recorded time is the absorption speed (unit: s).
Detailed description of the preferred embodiment 1
5 parts of decaalkyltrimethylammonium chloride and 95 parts of kaolin were put into a high-speed mixer and mixed at 2500rpm for 5 minutes to prepare an adsorbing material containing a deodorant. Adding 25.0kg of fine acrylic acid, 46.4kg of deionized water, 1.0kg of 10 wt% bridging agent polyethylene glycol 400 diacrylate, 0.25kg of deodorant-containing adsorbing material and 120g of octadecyl phosphate into a reaction kettle with a stirrer, uniformly mixing, cooling the reaction liquid to 15 ℃, and adding an initiator: 1.25kg of 1 wt% hydrogen peroxide and 0.60kg of 1 wt% ferrous sulfate. After the polymerization reaction is finished, the reactor is kept at 80 ℃ for 4 hours, then the colloid is extruded out of the reaction kettle and is crushed and granulated, and 23kg of 48 percent liquid caustic soda is added for neutralization during granulation. After granulation, the colloid is dried for 60min at 160 ℃, and the water content of the dried material is 3.8%. And crushing and screening the dried material to obtain a semi-finished product of the high-absorptivity resin with the particle size of 45-850 mu m. And treating the semi-finished product with a surface treatment solution to obtain a high-absorptivity resin finished product, wherein the surface treatment solution is prepared from ethylene glycol diglycidyl ether, butanediol, water and a radix sophorae flavescentis extract according to a ratio of 10:30:55:5, the dosage of the surface treatment solution is 3.0% of the mass of the SAP, the surface treatment temperature is 150 ℃, and the treatment time is 60 min.
Specific example 2
10 parts of methyltrihexadecyl ammonium bromide and 90 parts of activated carbon were put into a high-speed mixer and mixed at 2000rpm for 10 minutes to obtain an adsorbing material containing a deodorant. Adding 25.0kg of fine acrylic acid, 46.4kg of deionized water, 1.0kg of 10 wt% bridging agent polyethylene glycol 400 diacrylate, 0.3kg of deodorant-containing adsorbing material and 125g of octadecyl phosphate into a reaction kettle with a stirrer, uniformly mixing, cooling the reaction liquid to 15 ℃, and adding an initiator: 1.25kg of 1 wt% hydrogen peroxide and 0.60kg of 1 wt% ferrous sulfate. After the polymerization reaction is finished, the reactor is kept at 80 ℃ for 4 hours, then the colloid is extruded out of the reaction kettle and is crushed and granulated, and 23kg of 48 percent liquid caustic soda is added for neutralization during granulation. After granulation, the colloid is dried for 60min at 160 ℃, and the water content of the dried material is 3.5%. And crushing and screening the dried material to obtain a semi-finished product of the high-absorptivity resin with the particle size of 45-850 mu m. And treating the semi-finished product with a surface treatment solution to obtain a high-absorptivity resin finished product, wherein the surface treatment solution is prepared from ethylene glycol diglycidyl ether, butanediol, water and a thyme extract according to a ratio of 10:30:55:5, the dosage of the surface treatment solution is 3.0% of the mass of the SAP, the surface treatment temperature is 150 ℃, and the treatment time is 60 min.
Specific example 3
5 parts of decaalkyltrimethylammonium chloride and 95 parts of kaolin were put into a high-speed mixer and mixed at 2500rpm for 5 minutes to prepare an adsorbing material containing a deodorant. Adding 25.0kg of fine acrylic acid, 46.4kg of deionized water, 1.0kg of 10 wt% bridging agent polyethylene glycol 400 diacrylate, 0.25kg of deodorant-containing adsorbing material and 120g of octadecyl phosphate into a reaction kettle with a stirrer, uniformly mixing, cooling the reaction liquid to 15 ℃, and adding an initiator: 1.25kg of 1 wt% hydrogen peroxide and 0.60kg of 1 wt% ferrous sulfate. After the polymerization reaction is finished, the reactor is kept at 80 ℃ for 4 hours, then the colloid is extruded out of the reaction kettle and is crushed and granulated, and 23kg of 48 percent liquid caustic soda is added for neutralization during granulation. After granulation, the colloid is dried for 60min at 160 ℃, and the water content of the dried material is 3.4%. And crushing and screening the dried material to obtain a semi-finished product of the high-absorptivity resin with the particle size of 45-850 mu m. And treating the semi-finished product with a surface treatment solution to obtain a high-absorptivity resin finished product, wherein the surface treatment solution is prepared from ethylene glycol diglycidyl ether, butanediol, water and a cardamom extract according to a ratio of 10:30:50:10, the dosage of the surface treatment solution is 2.8% of the mass of the SAP, the surface treatment temperature is 150 ℃, and the treatment time is 60 min.
Specific example 4
8 parts of methyltrioctadecylammonium bromide and 92 parts of nano-silica were put into a high-speed mixer and mixed for 5 minutes at a rotation speed of 2800rpm to prepare an adsorbing material containing a deodorant. Adding 25.0kg of fine acrylic acid, 46.4kg of deionized water, 1.0kg of 10 wt% bridging agent polyethylene glycol 400 diacrylate, 0.28kg of deodorant-containing adsorbing material and 125g of octadecyl phosphate into a reaction kettle with a stirrer, uniformly mixing, cooling the reaction liquid to 15 ℃, and adding an initiator: 1.25kg of 1 wt% hydrogen peroxide and 0.60kg of 1 wt% ferrous sulfate. After the polymerization reaction is finished, the reactor is kept at 80 ℃ for 4 hours, then the colloid is extruded out of the reaction kettle and is crushed and granulated, and 23kg of 48 percent liquid caustic soda is added for neutralization during granulation. After granulation, the colloid is dried for 60min at 160 ℃, and the water content of the dried material is 3.6%. And crushing and screening the dried material to obtain a semi-finished product of the high-absorptivity resin with the particle size of 45-850 mu m. And treating the semi-finished product with a surface treatment solution to obtain a high-absorptivity resin finished product, wherein the surface treatment solution is prepared from ethylene glycol diglycidyl ether, butanediol, water and a radix sophorae flavescentis extract according to a ratio of 10:30:55:5, the dosage of the surface treatment solution is 3.0% of the mass of the SAP, the surface treatment temperature is 150 ℃, and the treatment time is 60 min.
Comparative example 1
Adding 25.0kg of fine acrylic acid, 46.4kg of deionized water and 1.0kg of 10 wt% of bridging agent polyethylene glycol 400 diacrylate into a reaction kettle with a stirrer, uniformly mixing, cooling the reaction liquid to 15 ℃, and adding an initiator: 1.25kg of 1 wt% hydrogen peroxide and 0.60kg of 1 wt% ferrous sulfate. After the polymerization reaction is finished, the reactor is kept at 80 ℃ for 4 hours, then the colloid is extruded out of the reaction kettle and is crushed and granulated, and 23kg of 48 percent liquid caustic soda is added for neutralization during granulation. After granulation, the colloid is dried for 60min at 160 ℃, and the water content of the dried material is 3.9%. And crushing and screening the dried material to obtain a semi-finished product of the high-absorptivity resin with the particle size of 45-850 mu m. And treating the semi-finished product with a surface treatment solution to obtain a high-absorptivity resin finished product, wherein the surface treatment solution is prepared from ethylene glycol diglycidyl ether, butanediol and water according to a ratio of 10:30:60, the dosage of the surface treatment solution is 3.0% of the mass of the SAP, the surface treatment temperature is 150 ℃, and the treatment time is 60 min.
The product performance of each specific example and comparative example. See table two for details.
Watch two
Example 1 Example 2 Example 3 Example 4 Comparative example 1
Removing odor grade of adult urine 1.4 1.3 1.5 1.2 4.5
Saline water absorption multiplying power g/g 59.0 60.0 61.0 60.6 62.5
Centrifugal water retention rate g/g 29.0 29.8 30.7 30.6 31.0
Absorbency under pressure 0.7psi g/g 23.7 23.0 23.4 22.9 21.9
Absorption speed/s 33 30 35 33 32
It should be noted that the technical features such as specific type selection of the reaction kettle and the like related to the present patent application should be regarded as the prior art, the specific structure, the operation principle, the control mode and the spatial arrangement mode of the technical features may be selected conventionally in the field, and should not be regarded as the invention point of the present patent, and the present patent is not further specifically described in detail.
It will be apparent to those skilled in the art that modifications and equivalents may be made in the embodiments and/or portions thereof without departing from the spirit and scope of the present invention.

Claims (10)

1. A method for preparing a high-absorptivity resin for removing adult urine odor is characterized by comprising the following steps:
a. acrylic acid, deionized water, a water-soluble initiator, a bridging agent, a dispersing agent and an adsorbing material containing a deodorant are polymerized in a reactor containing a stirring device to generate colloid;
b. the colloid formed in step a is crushed, granulated and neutralized with an alkaline substance, including but not limited to sodium hydroxide;
c. drying, crushing and screening the neutralized colloid to obtain a semi-finished product of the high-absorptivity resin for removing the odor of adult urine;
d. and c, treating the semi-finished product in the step c at a preset surface treatment temperature under the action of a surface cross-linking agent and a plant deodorant to obtain a finished product of the high-absorptivity resin for removing the adult urine smell.
2. The method for preparing a highly absorbent resin for removing adult urine as claimed in claim 1, wherein the absorbent material containing a deodorant is prepared by mixing a deodorant and an inorganic absorbent material at a high speed of 2000rpm and 0.1-10% of acrylic acid.
3. The method for preparing a highly absorbent resin for removing adult urine odor according to claim 1, wherein the deodorant is one or more selected from the group consisting of octyltrimethylammonium chloride, dodecyltrimethylammonium chloride, octylpyridinium chloride, dodecylpyridinium chloride, tetradecylpyridinium chloride, methyltridecamylammonium bromide, methyltridecylammonium chloride, methyltridecylammonium bromide, methyltridecylammonium chloride, and methyltridecylammonium bromide, and the amount of the deodorant is 0.01% to 25% of the adsorbent containing the deodorant.
4. The method for preparing a highly absorbent resin for removing adult urine odor as claimed in claim 2, wherein the inorganic adsorbent is selected from one or more of activated carbon, molecular sieve, zeolite, kaolin, silica sol, nano silica, nano carbon dioxide, and clay, and the amount of the inorganic adsorbent is 75% to 99.9% of the adsorbent containing the deodorant.
5. The method for preparing a super absorbent resin to remove odor of adult urine as claimed in claim 1, wherein the bridging agent is selected from one or more of pentaerythritol tetraacrylate, N' -methylenebisacrylamide, polyethylene glycol diacrylate, pentaerythritol triallyl ether, pentaerythritol triacrylate, and triallyl amine ester, and the amount of the bridging agent is 0.05% to 5% by mass of acrylic acid.
6. The method for preparing a super absorbent resin to remove odor of adult urine as claimed in claim 1, wherein the dispersant is one or more selected from sucrose fatty acid ester, octadecyl phosphate, monoglyceride, sorbitan monooleate, sorbitan tristearate, ethylene glycol distearate, castor oil/hydrogenated castor oil and ethylene oxide condensate, triglycerol monostearate, propylene glycol monostearate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, and carboxymethyl cellulose, and the amount of the dispersant is 0.001-1% by mass of acrylic acid.
7. The method for preparing a super absorbent resin for removing adult urine odor according to claim 1, wherein the surface cross-linking agent is one or more selected from ethanol, ethylene glycol, diethylene glycol, polyethylene glycol, glycerol, polyglycerol, isopropanol, 1, 4-butanediol, diethanolamine, triethanolamine, polyoxypropylene ether, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, and glycerol diglycidyl ether, and the amount of the surface cross-linking agent is 1% to 10% of the semi-finished product of the super absorbent resin for removing adult urine odor.
8. The method for preparing a super absorbent resin for removing adult urine according to claim 1, wherein the plant-type deodorant is one or more selected from thyme extract, sophora flavescens extract, cinnamon extract, senecio italica extract, mustard extract, horseradish extract, chitin extract, and cardamom extract, and the amount of the plant-type deodorant is 0.01-10% of the semi-finished product of the super absorbent resin for removing adult urine.
9. The method for preparing a super absorbent resin to remove odor of adult urine as claimed in claim 1, wherein the predetermined surface treatment temperature in the step d is 60-200 ℃.
10. A super absorbent resin for removing odor of adult urine, which is prepared by the method for preparing a super absorbent resin for removing odor of adult urine according to any one of claims 1 to 9.
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