CN109694441A - A kind of pearl high hydroscopic resin and preparation method thereof - Google Patents
A kind of pearl high hydroscopic resin and preparation method thereof Download PDFInfo
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- CN109694441A CN109694441A CN201710984422.0A CN201710984422A CN109694441A CN 109694441 A CN109694441 A CN 109694441A CN 201710984422 A CN201710984422 A CN 201710984422A CN 109694441 A CN109694441 A CN 109694441A
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- deionized water
- water
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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
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to a kind of pearl high hydroscopic resins and preparation method thereof, belong to resin technology field.The high hydroscopic resin includes water phase: acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters, ammonium persulfate, sodium hydrogensulfite, deionized water A, deionized water B, 10%NaOH；Oily phase: glycerine.The product is used in the form of bead, can largely be simplified the use process of water-absorbing resin, be extended the application range of water-absorbing resin.
Description
Technical field
The present invention relates to a kind of resins and preparation method thereof, it is more particularly related to a kind of pearl super absorbent resin
Rouge and preparation method thereof belongs to resin technology field.
Background technique
Super absorbent resin is a kind of new functional macromolecule material rapidly developed in recent years.It can absorb quality itself
Hundred times or even thousands of times of water, and have stronger water retention property.Thus in industry, agricultural, health care, daily life
Etc. be widely applied.
But the preparation of general high hydroscopic resin often uses bulk technique to produce, this result in production procedure compared with
Long, the disadvantages of postprocessing working procedures are more numerous.Directly significantly rise production cost, to greatly limit product
Popularization and application.Simultaneously as needing to carry out crushing to product and could use after bulk polymerization, production process is not only increased, together
When also cause in product crushing process and lose excessive, reduce the yield of product.
State Intellectual Property Office discloses a Publication No. CN102504288A, entitled " one kind in 2012.06.20
The invention of the preparation method of high hydroscopic resin ", the invention use radical polymerization initiator, in comprising surfactant and/or
In the petroleum hydrocarbon solvent of polymer protection colloid, in the presence of internal crosslinking agent, make water-soluble ethylenically unsaturated monomer into
Inverse suspension polymerization in row water-in-oil system, in polymerization reaction and last handling process addition containing Si-OH He ∕ or Si-O group
Substance, improve the performance of high hydroscopic resin.There is the high hydroscopic resin as made from the method for the present invention water holding capacity height, 1min to inhale
The features such as water absorbing capacity under physiological saline ability height, pressurization is high and rate of liquid aspiration is fast.
The above method prepares high hydroscopic resin and equally exists production and the high problem of product cost.
Summary of the invention
Present invention seek to address that high hydroscopic resin problem at high cost in the prior art, provides a kind of pearl super absorbent resin
Rouge, the high hydroscopic resin cost are significantly reduced.
In order to achieve the above-mentioned object of the invention, specific technical solution is as follows:
A kind of pearl high hydroscopic resin, it is characterised in that: including following raw materials in parts by weight:
Water phase:
Acrylic acid 40-45g
Hydroxyethyl methacrylate 5-10g
Dodecyl acrylate 3-5g
Double acrylic acid glycol ester 0.20-0.25g
Ammonium persulfate 0.30-0.50g
Sodium hydrogensulfite 0.30-0.50g
Deionized water A 50-80ml
Deionized water B 100-150ml
10%NaOH 100-120ml；
Oily phase:
Glycerine 400-500ml.
A kind of preparation method of pearl high hydroscopic resin, it is characterised in that: comprise the following steps that:
A, acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters are accurately weighed by water phase formula
In a beaker, it is thoroughly mixed uniformly, it is spare；
B, it is slowly added to 10% NaOH prepared using deionized water A under fast stirring, neutralization reaction is carried out to system；It is added
Deionized water B, stirs；
C, polymerization initiation system ammonium persulfate, sodium hydrogensulfite are prepared using deionized water A in another beaker, are sufficiently stirred
It is even, it is spare；
D, stirring is started, together with the glycerine measured is added in electric mixer, condenser pipe, feed opening there-necked flask one
When the system is warming up to 30-35 DEG C, it is spare；
E, it will be added to by the prepared polymerization initiation system of step C by step A in advance prepared reaction monomers mixture,
It is thoroughly mixed uniformly；
F, the ready polymeric monomer intermixture of step E is added in there-necked flask reactor；Electric stirring speed is adjusted, water is made
Phase reaction monomer system is dispersed in medium glycerol, until dispersion water phase grain diameter meets technique requirement；
G, temperature is risen to 50-55 DEG C in 0.5-1.0h；Suspension polymerization system starts polymerization reaction at 50-55 DEG C, dispersion
Bead starts to be changed into the solid particle for being able to maintain certain shapes by drop；By reaction temperature maintain 70-75 DEG C of heat preservation 5h,
2h, 85-90 DEG C of heat preservation 2h of 75-80 DEG C of heat preservation；
H, cooling, be filtered, washed, dry, sieving, packing.
Bring advantageous effects of the present invention:
High hydroscopic resin prepared by the present invention got rid of conventional bulk polymerization processes for preparing have to that resin crush etc. it is numerous
General labourer's sequence improves the yield of product, simplifies the production process of product, reduces the production cost of product.The product is with pearl
The form of body uses, and can largely simplify the use process of water-absorbing resin, extend the application range of water-absorbing resin.
Specific embodiment
Embodiment 1
A kind of pearl high hydroscopic resin, it is characterised in that: including following raw materials in parts by weight:
Water phase:
Acrylic acid 40g
Hydroxyethyl methacrylate 5g
Dodecyl acrylate 3g
Double acrylic acid glycol ester 0.20g
Ammonium persulfate 0.30g
Sodium hydrogensulfite 0.30g
Deionized water A 50ml
Deionized water B 100ml
10%NaOH 100ml；
Oily phase:
Glycerine 400ml.
Embodiment 2
A kind of pearl high hydroscopic resin, it is characterised in that: including following raw materials in parts by weight:
Water phase:
Acrylic acid 45g
Hydroxyethyl methacrylate 10g
Dodecyl acrylate 5g
Double acrylic acid glycol ester 0.25g
Ammonium persulfate 0.50g
Sodium hydrogensulfite 0.50g
Deionized water A 80ml
Deionized water B 150ml
10%NaOH 120ml；
Oily phase:
Glycerine 500ml.
Embodiment 3
A kind of pearl high hydroscopic resin, it is characterised in that: including following raw materials in parts by weight:
Water phase:
Acrylic acid 42.5g
Hydroxyethyl methacrylate 7.5g
Dodecyl acrylate 4g
Double acrylic acid glycol ester 0.225g
Ammonium persulfate 0.4g
Sodium hydrogensulfite 0.4g
Deionized water A 65ml
Deionized water B 125ml
10%NaOH 110ml；
Oily phase:
Glycerine 450ml.
Embodiment 4
A kind of pearl high hydroscopic resin, it is characterised in that: including following raw materials in parts by weight:
Water phase:
Acrylic acid 42g
Hydroxyethyl methacrylate 8g
Dodecyl acrylate 3.5g
Double acrylic acid glycol ester 0.21g
Ammonium persulfate 0.32g
Sodium hydrogensulfite 0.46g
Deionized water A 66ml
Deionized water B 111ml
10%NaOH 109ml；
Oily phase:
Glycerine 420ml.
Embodiment 5
A kind of preparation method of pearl high hydroscopic resin, it is characterised in that: comprise the following steps that:
A, acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters are accurately weighed by water phase formula
In a beaker, it is thoroughly mixed uniformly, it is spare；
B, it is slowly added to 10% NaOH prepared using deionized water A under fast stirring, neutralization reaction is carried out to system；It is added
Deionized water B, stirs；
C, polymerization initiation system ammonium persulfate, sodium hydrogensulfite are prepared using deionized water A in another beaker, are sufficiently stirred
It is even, it is spare；
D, stirring is started, together with the glycerine measured is added in electric mixer, condenser pipe, feed opening there-necked flask one
When the system is warming up to 30 DEG C, it is spare；
E, it will be added to by the prepared polymerization initiation system of step C by step A in advance prepared reaction monomers mixture,
It is thoroughly mixed uniformly；
F, the ready polymeric monomer intermixture of step E is added in there-necked flask reactor；Electric stirring speed is adjusted, water is made
Phase reaction monomer system is dispersed in medium glycerol, until dispersion water phase grain diameter meets technique requirement；
G, temperature is risen to 50 DEG C in 0.5h；Suspension polymerization system starts polymerization reaction at 50 DEG C, dispersion bead start by
Drop is changed into the solid particle for being able to maintain certain shapes；Reaction temperature is maintained into 70 DEG C of heat preservation 5h, 75 DEG C of heat preservation 2h, 85 DEG C
Keep the temperature 2h；
H, cooling, be filtered, washed, dry, sieving, packing.
Embodiment 6
A kind of preparation method of pearl high hydroscopic resin, it is characterised in that: comprise the following steps that:
A, acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters are accurately weighed by water phase formula
In a beaker, it is thoroughly mixed uniformly, it is spare；
B, it is slowly added to 10% NaOH prepared using deionized water A under fast stirring, neutralization reaction is carried out to system；It is added
Deionized water B, stirs；
C, polymerization initiation system ammonium persulfate, sodium hydrogensulfite are prepared using deionized water A in another beaker, are sufficiently stirred
It is even, it is spare；
D, stirring is started, together with the glycerine measured is added in electric mixer, condenser pipe, feed opening there-necked flask one
When the system is warming up to 35 DEG C, it is spare；
E, it will be added to by the prepared polymerization initiation system of step C by step A in advance prepared reaction monomers mixture,
It is thoroughly mixed uniformly；
F, the ready polymeric monomer intermixture of step E is added in there-necked flask reactor；Electric stirring speed is adjusted, water is made
Phase reaction monomer system is dispersed in medium glycerol, until dispersion water phase grain diameter meets technique requirement；
G, temperature is risen to 55 DEG C in 1.0h；Suspension polymerization system starts polymerization reaction at 55 DEG C, dispersion bead start by
Drop is changed into the solid particle for being able to maintain certain shapes；Reaction temperature is maintained into 75 DEG C of heat preservation 5h, 80 DEG C of heat preservation 2h, 90 DEG C
Keep the temperature 2h；
H, cooling, be filtered, washed, dry, sieving, packing.
Embodiment 7
A kind of preparation method of pearl high hydroscopic resin, it is characterised in that: comprise the following steps that:
A, acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters are accurately weighed by water phase formula
In a beaker, it is thoroughly mixed uniformly, it is spare；
B, it is slowly added to 10% NaOH prepared using deionized water A under fast stirring, neutralization reaction is carried out to system；It is added
Deionized water B, stirs；
C, polymerization initiation system ammonium persulfate, sodium hydrogensulfite are prepared using deionized water A in another beaker, are sufficiently stirred
It is even, it is spare；
D, stirring is started, together with the glycerine measured is added in electric mixer, condenser pipe, feed opening there-necked flask one
When the system is warming up to 32.5 DEG C, it is spare；
E, it will be added to by the prepared polymerization initiation system of step C by step A in advance prepared reaction monomers mixture,
It is thoroughly mixed uniformly；
F, the ready polymeric monomer intermixture of step E is added in there-necked flask reactor；Electric stirring speed is adjusted, water is made
Phase reaction monomer system is dispersed in medium glycerol, until dispersion water phase grain diameter meets technique requirement；
G, temperature is risen to 52.5 DEG C in 0.75h；Suspension polymerization system starts polymerization reaction at 52.5 DEG C, and dispersion bead is opened
Beginning is changed into the solid particle for being able to maintain certain shapes by drop；Reaction temperature is maintained into 72.5 DEG C of heat preservation 5h, 77.5 DEG C of guarantors
Warm 2h, 87.5 DEG C of heat preservation 2h；
H, cooling, be filtered, washed, dry, sieving, packing.
Embodiment 8
A kind of preparation method of pearl high hydroscopic resin, it is characterised in that: comprise the following steps that:
A, acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters are accurately weighed by water phase formula
In a beaker, it is thoroughly mixed uniformly, it is spare；
B, it is slowly added to 10% NaOH prepared using deionized water A under fast stirring, neutralization reaction is carried out to system；It is added
Deionized water B, stirs；
C, polymerization initiation system ammonium persulfate, sodium hydrogensulfite are prepared using deionized water A in another beaker, are sufficiently stirred
It is even, it is spare；
D, stirring is started, together with the glycerine measured is added in electric mixer, condenser pipe, feed opening there-necked flask one
When the system is warming up to 32 DEG C, it is spare；
E, it will be added to by the prepared polymerization initiation system of step C by step A in advance prepared reaction monomers mixture,
It is thoroughly mixed uniformly；
F, the ready polymeric monomer intermixture of step E is added in there-necked flask reactor；Electric stirring speed is adjusted, water is made
Phase reaction monomer system is dispersed in medium glycerol, until dispersion water phase grain diameter meets technique requirement；
G, temperature is risen to 53 DEG C in 0.55h；Suspension polymerization system starts polymerization reaction at 53 DEG C, dispersion bead start by
Drop is changed into the solid particle for being able to maintain certain shapes；Reaction temperature is maintained into 71 DEG C of heat preservation 5h, 78 DEG C of heat preservation 2h, 88 DEG C
Keep the temperature 2h；
H, cooling, be filtered, washed, dry, sieving, packing.
Claims (2)
1. a kind of pearl high hydroscopic resin, it is characterised in that: including following raw materials in parts by weight:
Water phase:
Acrylic acid 40-45g
Hydroxyethyl methacrylate 5-10g
Dodecyl acrylate 3-5g
Double acrylic acid glycol ester 0.20-0.25g
Ammonium persulfate 0.30-0.50g
Sodium hydrogensulfite 0.30-0.50g
Deionized water A 50-80ml
Deionized water B 100-150ml
10%NaOH 100-120ml；
Oily phase:
Glycerine 400-500ml.
2. a kind of preparation method of pearl high hydroscopic resin according to claim 1, it is characterised in that: including following technique
Step:
A, acrylic acid, hydroxyethyl methacrylate, dodecyl acrylate, double acrylic acid glycol esters are accurately weighed by water phase formula
In a beaker, it is thoroughly mixed uniformly, it is spare；
B, it is slowly added to 10% NaOH prepared using deionized water A under fast stirring, neutralization reaction is carried out to system；It is added
Deionized water B, stirs；
C, polymerization initiation system ammonium persulfate, sodium hydrogensulfite are prepared using deionized water A in another beaker, are sufficiently stirred
It is even, it is spare；
D, stirring is started, together with the glycerine measured is added in electric mixer, condenser pipe, feed opening there-necked flask one
When the system is warming up to 30-35 DEG C, it is spare；
E, it will be added to by the prepared polymerization initiation system of step C by step A in advance prepared reaction monomers mixture,
It is thoroughly mixed uniformly；
F, the ready polymeric monomer intermixture of step E is added in there-necked flask reactor；Electric stirring speed is adjusted, water is made
Phase reaction monomer system is dispersed in medium glycerol, until dispersion water phase grain diameter meets technique requirement；
G, temperature is risen to 50-55 DEG C in 0.5-1.0h；Suspension polymerization system starts polymerization reaction at 50-55 DEG C, dispersion
Bead starts to be changed into the solid particle for being able to maintain certain shapes by drop；By reaction temperature maintain 70-75 DEG C of heat preservation 5h,
2h, 85-90 DEG C of heat preservation 2h of 75-80 DEG C of heat preservation；
H, cooling, be filtered, washed, dry, sieving, packing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710984422.0A CN109694441A (en) | 2017-10-20 | 2017-10-20 | A kind of pearl high hydroscopic resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710984422.0A CN109694441A (en) | 2017-10-20 | 2017-10-20 | A kind of pearl high hydroscopic resin and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481434A (en) * | 2009-01-22 | 2009-07-15 | 潍坊中石科技有限公司 | Method for preparing big particle pearl-like water absorption resin, resin prepared thereby and preparing apparatus |
| CN103130942A (en) * | 2011-11-22 | 2013-06-05 | 范立涛 | Preparation method of spherical water-absorbent resin and cold warm compress product thereof |
| CN105294919A (en) * | 2015-12-08 | 2016-02-03 | 中蓝晨光化工研究设计院有限公司 | Post-crosslinking super absorbent resin and preparation method thereof |
| CN106674414A (en) * | 2017-01-19 | 2017-05-17 | 中蓝晨光化工研究设计院有限公司 | Acrylic resin and preparation method thereof |
-
2017
- 2017-10-20 CN CN201710984422.0A patent/CN109694441A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481434A (en) * | 2009-01-22 | 2009-07-15 | 潍坊中石科技有限公司 | Method for preparing big particle pearl-like water absorption resin, resin prepared thereby and preparing apparatus |
| CN103130942A (en) * | 2011-11-22 | 2013-06-05 | 范立涛 | Preparation method of spherical water-absorbent resin and cold warm compress product thereof |
| CN105294919A (en) * | 2015-12-08 | 2016-02-03 | 中蓝晨光化工研究设计院有限公司 | Post-crosslinking super absorbent resin and preparation method thereof |
| CN106674414A (en) * | 2017-01-19 | 2017-05-17 | 中蓝晨光化工研究设计院有限公司 | Acrylic resin and preparation method thereof |
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Application publication date: 20190430 |
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