CN103788315A - Preparation method for amphoteric water-in-oil inverse emulsion - Google Patents
Preparation method for amphoteric water-in-oil inverse emulsion Download PDFInfo
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- CN103788315A CN103788315A CN201410018098.3A CN201410018098A CN103788315A CN 103788315 A CN103788315 A CN 103788315A CN 201410018098 A CN201410018098 A CN 201410018098A CN 103788315 A CN103788315 A CN 103788315A
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Abstract
The invention discloses a preparation method for amphoteric water-in-oil inverse emulsion. The preparation method comprises the following steps: respectively adding a non-ion monomer, an anion monomer, a cation monomer, a water quality stabilizer and a molecular weight modifier into water; adjusting PH (Potential of Hydrogen) to obtain a water phase A and a water phase B with different ratios; adding a non-ion emulsifying agent into a hydrocarbons solvent to prepare an oil phase; dividing the oil phase into two parts; respectively dropwise adding the water phase A and the water phase B into the two parts of the oil phase; carrying out one-step emulsification or multi-step emulsification to obtain emulsion A and emulsion B; displacing the emulsion A and the emulsion B by using insert gas to remove oxygen; adjusting the temperature of the emulsion B to an initiation temperature; adding an initiator and after polymerization is carried out for 30-120 minutes, dropwise adding the emulsion A; continually reacting to convert all the monomers into polymers; and finishing the reaction to obtain an amphoteric water-in-oil inverse emulsion product. Amphoteric polyacrylamide prepared by the preparation method has different molecular structures, also has the advantages of high effective content, high molecular weight, low viscosity and can be dissolved quickly.
Description
Technical field:
The present invention relates to a kind of preparation method of multipolymer, particularly a kind of preparation method of both sexes water-in-oil reversed-phase emulsion
Background technology:
Normal by adding some auxiliary agents in order to improve the pi of strength of paper in paper technology, Dry Strength Resin is the more important auxiliary agent of one of them usage quantity.Dry Strength Resin is for tensile strength, tear strength, bursting strength and folding endurance and the deflection of paper under dry state is provided, its Main Function is internal bond between fortifying fibre, many water miscible, the superpolymer that can form hydrogen bonded with fiber can become Dry Strength Resin.Study of Paper-Strengthening Agent Based has two kinds of natural polymer and modifier thereof and synthetic polymers, in natural polymer, is mainly wherein starch and modifier thereof.Starch and modifier thereof be in source, have a some superiority in price, but its large usage quantity in general, and the reinforced effects obtaining is not good enough, and this class Dry Strength Resin can cause paper machine dewatering speed to reduce, and affect paper and normally produce, and increases energy consumption while being dried.Comparatively speaking, synthetic polymer has more handiness in structure and molecular weight, substituent control, thereby use range is wider, reinforced effects is expected to better.If paper is dry strong with synthetic polymeric main polyacrylamide, comprise anionic, cationic and both sexes product.
The modal product form of amphiprotic polyacrylamide of using as Dry Strength Resin is at present aqueous solution type.There is obvious advantage with aqueous process polymerization, the preparation of aqueous solution polymerization system easily, polymerization process control is simple, its method is substantially as follows: by water-soluble monomer, (comprising acrylamide, cationic monomer, anionic monomer etc.), water quality stabilizer, deionized water are configured to the aqueous solution, regulate pH to certain limit, after nitrogen replacement, rise to certain temperature, add initiator initiated polymerization to obtain amphiprotic polyacrylamide product.For example Chemical Engineering Institute, HangZhou City discloses a kind of Dry Strength Resin preparation method who contains sulfonic acid or phosphate group in state's patent CN1388288A therein, in flask, first water miscible monomer (such as acrylamide, acrylamide group methyl propanesulfonic acid, methacryloyl amido propyl ester trimethyl ammonium chloride etc.) is dissolved in water, initiator is mixed with to the aqueous solution, after being warming up to 80 degree, start to drip initiator solution, after reaction, obtain amphiprotic polyacrylamide product, product solids content 16%, the about 7500mPa.s of viscosity.
In order to control viscosity or the molecular weight of product, the effective content of amphiprotic polyacrylamide product is controlled at 15～20wt% conventionally, and molecular weight is also controlled at 500,000 left and right.In the time controlling molecular weight, use molecular weight regulator more, also utilize polymerization technique control, take to drip the mode of monomer, in the hierarchy of control, monomer concentration, in lower level, to obtain lower molecular weight products, is avoided causing product viscosity too high because molecular weight product is too high.
Summary of the invention:
The present invention seeks to, be used for making up the deficiencies in the prior art, and the preparation method of the both sexes water-in-oil reversed-phase emulsion of a kind of high effective content, high molecular is provided.
To achieve these goals, technical scheme of the present invention is as follows:
A preparation method for both sexes water-in-oil reversed-phase emulsion, comprises following step:
(1) non-ionic monomer, anionic monomer, cationic monomer, water quality stabilizer, molecular weight regulator are added to the water, regulate PH=5.0-10.0, configuration obtains water, be 9:1-1:2 by the mass ratio of cationic monomer in water and anionic monomer, preferred proportion is 4:1-1:1, obtains water A; Be 2:1-1:9 by the mass ratio of cationic monomer and anionic monomer, preferred proportion is 1:1-1:4, obtains aqueous phase B;
(2) nonionic emulsifying agent is added and in varsol, be configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through a step emulsification or multistep emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add initiator initiated polymerization, after polyase 13 0-120min, start to drip latex A, continue reaction and make all conversion of monomers become polymerization, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
Described non-ionic monomer is selected from one or more in following substances: acrylamide, Methacrylamide, N,N-DMAA, Dimethylaminoethyl Methacrylate, Hydroxyethyl acrylate or NVP
Described anionic monomer is selected from one or more in following substances: vinylformic acid, methacrylic acid, propenyl sulfonic acid, 2-acrylamide-2-methylpro panesulfonic acid, vinylbenzenesulfonic acid, toxilic acid, maleic anhydride or contain carboxylic acid group or all or part of salt being neutralized into of sulfonic anionic monomer; The alkali that neutralization is used is ammoniacal liquor, sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood or sodium bicarbonate; Degree of neutralization in molar ratio percentage composition meter accounts for 50mol%-100mol%, is preferably 70%-100%.
Described cationic monomer is selected from one or more in following substances: acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamido oxypropyl trimethyl ammonium chloride, methacryloyl amido propyl group ammonio methacrylate or diallyldimethylammonium chloride.
The use total amount of described non-ionic monomer, anionic monomer and cationic monomer accounts for the 10%-60% of both sexes water-in-oil reversed-phase emulsion total mass, is preferably 15%-50%, more preferably 25%-45%; The mass ratio of described non-ionic monomer and zwitterion monomer is 1:19～19:1, is preferably 1:4-4:1.
Described water quality stabilizer is sequestrant; The consumption of sequestrant is the 0.005%-0.1% of water quality.
Described sequestrant is disodium edta or diethylene triamine pentacetic acid (DTPA) five sodium-salt.
Described molecular weight regulator is the water-soluble substances with chain transfer; The consumption of molecular weight regulator is no more than 2% of the both sexes water-in-oil reversed-phase emulsion total mass preparing.
Lower aliphatic alcohols, mercaptan, formate, methallylsulfonic acid sodium or urea that the described water-soluble substances with chain transfer is C1-C4.
Described varsol is the saturated or unsaturated hydrocarbons of C6-C30; The usage quantity of varsol is the 10%-50% of both sexes water-in-oil reversed-phase emulsion total mass, is preferably 15%-25%.
Described emulsifying agent is nonionic emulsifying agent, and its hydrophile-lipophile balance value is 2.0-15.0; The consumption of emulsifying agent is the 1%-15% of both sexes water-in-oil reversed-phase emulsion total mass, is preferably 2-10%.
Described nonionic emulsifying agent is selected from one or more in following substances: sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, aliphatic alcohol polyethenoxy base ether, sorbyl alcohol glycidyl ether, polyoxyethylene carboxylate, alkylphenol-polyethenoxy base ether or aromatic series polyoxyethylene ether.
Described initiator is initiator, the peroxide initiator that contains azo group or the redox initiator being made up of Oxidizing and Reducing Agents; Initiator amount is the 0.001%-0.1% of both sexes water-in-oil reversed-phase emulsion total mass.
The described initiator that contains azo group is azo di-isopropyl imidazoline salt hydrochlorate, azo diisobutyl amidine hydrochloride or Diisopropyl azodicarboxylate; Described peroxide initiator is hydrogen peroxide, dibenzoyl peroxide or tertbutyl peroxide; In the described redox initiator being made up of Oxidizing and Reducing Agents, oxygenant is selected from one or more in following substances: persulphate, bromate or superoxide; In the described redox initiator being made up of Oxidizing and Reducing Agents, reductive agent is selected from one or more in following substances: sulphite, lay particular stress on sulphite, thiosulphate, Fe
2+, Cu
+or organic amine.
Described initiator is the redox initiator being made up of Oxidizing and Reducing Agents, when it uses, first adds described oxygenant in water, after mixing and emulsifying, adds described reductive agent when polymerization again, and the consumption of oxygenant and reductive agent is 1:2-2:1.
Described oxygenant is selected from one or more in following substances: Sodium Persulfate, ammonium persulphate, Potassium Persulphate, sodium bromate, potassium bromate, hydrogen peroxide, tertbutyl peroxide or dibenzoyl peroxide; Described reductive agent is selected from one or more in following substances: S-WAT, sodium bisulfite, Sodium Metabisulfite, Sulfothiorine, V-Brite B, iron protochloride, ferrous sulfate, cuprous chloride, triethylamine, trolamine or Tetramethyl Ethylene Diamine.
Beneficial effect of the present invention is as follows:
The amphiprotic polyacrylamide that the present invention prepares has inhomogenous molecular structure, has high effective content simultaneously, high molecular, low viscosity, rapidly-soluble advantage.This polymeric articles molecular structure heterogeneity is more suitable for the enhancing of complicated paste system in the time of application; Effective content is high, is convenient to the transportation of product stock, saves transportation cost; Molecular weight is high, is conducive to removing of paper-making process water; Product viscosity is low, is convenient to carry in use procedure; Dissolution rate can be saved dissolution equipment investment soon.
Embodiment:
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
(1) acrylamide, toxilic acid, acrylyl oxy-ethyl-trimethyl salmiac, disodium edta, mercaptan are added to the water, regulate PH=5.0, configuration obtains water A, and wherein the mass ratio of acrylyl oxy-ethyl-trimethyl salmiac and toxilic acid is 9:1;
Acrylamide, toxilic acid, acrylyl oxy-ethyl-trimethyl salmiac, disodium edta, mercaptan are added to the water, regulate PH=10.0, configuration obtains aqueous phase B, wherein the mass ratio of acrylyl oxy-ethyl-trimethyl salmiac and toxilic acid is 1:9, and the mass ratio of water A and aqueous phase B is 4:6;
(2) polyoxyethylene carboxylate is added and in cyclohexane solvent, be configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through a step emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add azo diisobutyl amidine hydrochloride initiated polymerization, after polyase 13 0min, start to drip latex A, continue reaction and make all conversion of monomers become polymerization, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
The use total amount of described acrylamide, toxilic acid and acrylyl oxy-ethyl-trimethyl salmiac accounts for 33% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of disodium edta is 0.1% of water quality; The consumption of mercaptan is 0.018% of the both sexes water-in-oil reversed-phase emulsion total mass for preparing.The usage quantity of cyclohexane solvent is 30% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of polyoxyethylene carboxylate is 10% of both sexes water-in-oil reversed-phase emulsion total mass.Azo diisobutyl amidine hydrochloride consumption is 0.1% of both sexes water-in-oil reversed-phase emulsion total mass.
Embodiment 2
(1) Methacrylamide, 2-acrylamide-2-methylpro panesulfonic acid, methacryloyl amido oxypropyl trimethyl ammonium chloride, diethylene triamine pentacetic acid (DTPA) sodium salt, sodium formiate are added to the water, regulate PH=6.0, configuration obtains water A, and wherein the mass ratio of methacryloyl amido oxypropyl trimethyl ammonium chloride and 2-acrylamide-2-methylpro panesulfonic acid is 4:1;
Methacrylamide, 2-acrylamide-2-methylpro panesulfonic acid, methacryloyl amido oxypropyl trimethyl ammonium chloride, diethylene triamine pentacetic acid (DTPA) sodium salt, sodium formiate are added to the water, regulate PH=8.0, configuration obtains aqueous phase B, and wherein the mass ratio of methacryloyl amido oxypropyl trimethyl ammonium chloride and 2-acrylamide-2-methylpro panesulfonic acid is 1:6; The mass ratio of water A and aqueous phase B is 3:7
(2) sorbitan fatty acid ester and polyoxyethylene sorbitan fatty acid ester (the two part by weight is 8:1) are added in 7# white oil and be configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through multistep emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add ammonium persulphate and bisulfite sodium polymerization, after polymerization 120min, start to drip latex A, continue reaction and make all conversion of monomers become polymerization, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
The use total amount of described Methacrylamide, 2-acrylamide-2-methylpro panesulfonic acid and methacryloyl amido oxypropyl trimethyl ammonium chloride accounts for 40% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of diethylene triamine pentacetic acid (DTPA) sodium salt is 0.009% of water quality; The consumption of sodium formiate is 1% of the both sexes water-in-oil reversed-phase emulsion total mass for preparing.The usage quantity of 7# white oil is 28% of both sexes water-in-oil reversed-phase emulsion total mass; Total consumption of sorbitan fatty acid ester and polyoxyethylene sorbitan fatty acid ester is 2% of both sexes water-in-oil reversed-phase emulsion total mass.Ammonium persulphate consumption is 0.001% of both sexes water-in-oil reversed-phase emulsion total mass, and the consumption of sodium bisulfite is 0.0015% of both sexes water-in-oil reversed-phase emulsion total mass.
Embodiment 3
(1) Hydroxyethyl acrylate, vinylformic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, diethylene triamine pentacetic acid (DTPA) five sodium-salt, sodium formiate are added to the water, regulate PH=7.0, configuration obtains water, is 5:1 by the mass ratio of cationic monomer in water and anionic monomer, obtains water A; Be that 1:4 obtains aqueous phase B by the mass ratio of cationic monomer and anionic monomer; The mass ratio of water A and aqueous phase B is 7:3
(2) alkylphenol-polyethenoxy base ether is added and in toluene, be configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through a step emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add Diisopropyl azodicarboxylate, after polymerization 45min, start to drip latex A, continue reaction and make all conversion of monomers become polymerization, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
The use total amount of described Hydroxyethyl acrylate, vinylformic acid and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride accounts for 15% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of diethylene triamine pentacetic acid (DTPA) five sodium-salt is 0.005% of water quality; The consumption of sodium formiate is 0.2% of the both sexes water-in-oil reversed-phase emulsion total mass for preparing.The usage quantity of toluene is 26% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of alkylphenol-polyethenoxy base ether is 7% of both sexes water-in-oil reversed-phase emulsion total mass.The consumption of Diisopropyl azodicarboxylate is 0.005% of both sexes water-in-oil reversed-phase emulsion total mass.
Embodiment 4
(1) Dimethylaminoethyl Methacrylate, vinylbenzenesulfonic acid, diallyldimethylammonium chloride, disodium edta, methallylsulfonic acid sodium are added to the water, regulate PH=7.0, configuration obtains water A, and wherein the mass ratio of diallyldimethylammonium chloride and maleic anhydride is 1:2.
Dimethylaminoethyl Methacrylate, vinylbenzenesulfonic acid, diallyldimethylammonium chloride, disodium edta, methallylsulfonic acid sodium are added to the water, regulate PH=9.0, configuration obtains aqueous phase B, and wherein the mass ratio of diallyldimethylammonium chloride and vinylbenzenesulfonic acid is 2:1; The mass ratio of water A and aqueous phase B is 3:7
(2) polyoxyethylene sorbitan fatty acid ester is added and in whiteruss, be configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through a step emulsification or multistep emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add azo di-isopropyl imidazoline salt hydrochlorate initiated polymerization, after polymerization 50min, start to drip latex A, continue reaction and make all conversion of monomers become polymerization, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
The use total amount of described Dimethylaminoethyl Methacrylate, vinylbenzenesulfonic acid and diallyldimethylammonium chloride accounts for 25% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of disodium edta is 0.05% of water quality; The consumption of methallylsulfonic acid sodium is 0.5% of the both sexes water-in-oil reversed-phase emulsion total mass for preparing.The usage quantity of whiteruss is 20% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of polyoxyethylene sorbitan fatty acid ester is 5% of both sexes water-in-oil reversed-phase emulsion total mass.Azo di-isopropyl imidazoline salt hydrochlorate consumption is 0.02% of both sexes water-in-oil reversed-phase emulsion total mass.
Embodiment 5
(1) acrylamide, vinylformic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, disodium ethylene diamine tetraacetate, urea are added to the water, regulate PH=7.0, configuration obtains water, is 3:1 by the mass ratio of cationic monomer in water and anionic monomer, obtains water A;
Acrylamide, vinylformic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, disodium ethylene diamine tetraacetate, urea are added to the water, regulate PH=7.0, configuration obtains water, is that 1:6 obtains aqueous phase B by the mass ratio of cationic monomer and anionic monomer, adds Sodium Persulfate in water; The mass ratio of water A and aqueous phase B is 6:4.
(2) sorbyl alcohol glycidyl ester ether is added in 5# white mineral oil and is configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through a step emulsification or multistep emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add SODIUM HYDROSULPHITE sodium polymerization, after polymerization 60min, start to drip latex A, continue reaction and make all conversion of monomers become polymerization, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
The use total amount of described acrylamide, vinylformic acid and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride accounts for 40% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of disodium ethylene diamine tetraacetate is 0.05% of water quality; The consumption of urea is 0.5% of the both sexes water-in-oil reversed-phase emulsion total mass for preparing.The usage quantity of 5# white mineral oil is 25% of both sexes water-in-oil reversed-phase emulsion total mass; The consumption of sorbyl alcohol glycidyl ester ether is 3% of both sexes water-in-oil reversed-phase emulsion total mass.Sodium Persulfate and V-Brite B consumption are 0.02% of both sexes water-in-oil reversed-phase emulsion total mass, and the consumption of Sodium Persulfate and V-Brite B is 1:2.
Performance test and result
Make up a prescription
Medicament: Tai-Ace S 150, positively charged ion pressed powder retention filtration adjuvant (hereinafter to be referred as cationic retention aid agent), the prepared amphiprotic polyacrylamide water-in-oil reversed-phase emulsion (hereinafter to be referred as emulsion drying strengthening agent) of the present invention
Tai-Ace S 150: Aluminium Sulphate usp (powder) (analytical pure) is configured to 5% aqueous solution stand-by;
Cationic retention aid agent: cationic retention aid agent powder is configured to 0.1% aqueous solution stand-by;
Emulsion drying strengthening agent: emulsion drying strengthening agent is configured to 0.5% aqueous solutions of polymers according to monomer content stand-by.
1, making beating
Raw material: disregard message paper, on-the-spot paper waste, boxboard etc.
Required instrument: balance, hollander, platform scale, Schooper-Riegler beating degree tester, plastic cup, Water Tank with Temp.-controlled, 1L graduated cylinder
Operation steps: weigh in the balance and get the on-the-spot paper waste of 200g, adding is 4 premium on currency, puts at twice fiber dissociation device and dissociates and 3000 turn, and then places and soaks 1h.Paper pulp after soaking is poured in hollander, added 16kg water to be made into 1% slurry.Dissociate and pull an oar with hollander.Within every 2 minutes, survey a beating degree, until making beating is to 25 degree.
The mensuration of beating degree is according to GB/T3332-2004 method.
2, the configuration of slurry
Required instrument: platform scale, 60kg plastic tank, aeration board, air compressor machine
Operation steps: the slurry of having beaten in hollander is transferred in the plastic tank of 60kg, is diluted to 0.8% concentration with clear water.Put into aeration board, aeration agitation slurry is stand-by.
3, the detection of Dry Strength Resin drainage rate
Required instrument: DFR-05 dynamic drainage freeness retains instrument
Operation steps: pack drainage test module into DFR-05 main frame.Open DFR-05 application program, and enter Drainage interface.
Parameter setting: forming net: 60 orders stop setting: 60S or 800g
Stirring velocity is set: front 10S, 10S after 700R/min, 800R/min
speedduringfiltration:0rpm
Chemical feeding points and chemical feeding quantity: 10S adds emulsion drying strengthening agent, chemical feeding quantity is 25kg/ ton slurry.
The slurry that takes 1000g0.8% adds in DFR-05, and the emulsion drying strengthening agent aqueous solution that pipettes 4ml2% with liquid-transfering gun is put into chemicals dosing plant, clicks " beginning " key and starts drainage rate mensuration.
4, adding and handsheet of medicament
Required instrument: beaker, transfer pipet, balance, four leaf agitators, stopwatch, pattern handshcet former
Operation steps: take the slurry of 500g0.8% in beaker, place on four leaf agitators and stir, by on-the-spot paper machine chemical feeding quantity and order, add successively reagent (after opening agitator, to start timing with transfer pipet, when 10S, add 5% Tai-Ace S 150 2ml, when 20S, add 2% emulsion drying strengthening agent 2ml, when 50S, add 0.1% cationic retention aid agent 2ml, when 80S, stop stirring, take off slurry and be transferred to handsheet in pattern handshcet former.
5, squeezing
Required instrument: pattern squeezing machine
Operation steps: pattern on pattern handshcet former is moved in pattern squeezing machine, open electric motor starting button, press push button rammer board and start to move down, squeezing 20S, presses rising button, and rammer board is mentioned.
6, dry
Required instrument: the flat pattern flash dryer of PL7-B type
Operation steps: open pattern flash dryer preheating number minute, temperature is adjusted to 95 ℃.Pattern in squeezing machine is moved in moisture eliminator, cover cover plate until pattern is dried.
7, fixed temperature and humidity
Operation steps: pattern after oven dry is moved in constant-temperature constant-humidity environment.
9, cutting of pattern
Required instrument: standard scudding knife
Operation steps: the pattern of fixed temperature and humidity processing is cut into appointment length and width with standard scudding knife, for the detection of paper below.
10, the detection of paper strength performance
Required instrument: paper bursting strength instrument, ring are pressed instrument, folding endurance instrument, electronic tearability instrument, tensile strength instrument, interlaminar strength instrument
Operation steps: in strict accordance with GB and the operation of instrument operation instruction.
Result:
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (17)
1. a preparation method for both sexes water-in-oil reversed-phase emulsion, is characterized in that, comprises following step:
(1) non-ionic monomer, anionic monomer, cationic monomer, water quality stabilizer, molecular weight regulator are added to the water, regulate pH=5.0-10.0, configuration obtains water, is 9:1-1:2 by the mass ratio of cationic monomer in water and anionic monomer, obtains water A; Be that 2:1-1:9 obtains aqueous phase B by the mass ratio of cationic monomer and anionic monomer;
(2) nonionic emulsifying agent is added and in varsol, be configured to oil phase; Oil phase is divided into two portions, water A and B are splashed into respectively in oil phase, obtain two kinds of latex A and emulsion B through a step emulsification or multistep emulsification;
(3) latex A and emulsion B are used respectively to inert gas replacement deoxygenation, emulsion B temperature is adjusted to kick off temperature, add initiator initiated polymerization, after polyase 13 0-120min, start to drip latex A, continue reaction and make all conversion of monomers become polymkeric substance, reaction finishes to obtain both sexes water-in-oil reversed-phase emulsion product.
2. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, is characterized in that, in water A, the mass ratio of cationic monomer and anionic monomer is 4:1-1:1; In aqueous phase B, the mass ratio of cationic monomer and anionic monomer is 1:1-1:4.
3. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, it is characterized in that, described non-ionic monomer is selected from one or more in following substances: acrylamide, Methacrylamide, N,N-DMAA, Dimethylaminoethyl Methacrylate, Hydroxyethyl acrylate or NVP.
4. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, it is characterized in that, described anionic monomer is selected from one or more in following substances: vinylformic acid, methacrylic acid, propenyl sulfonic acid, 2-acrylamide-2-methylpro panesulfonic acid, vinylbenzenesulfonic acid, toxilic acid, maleic anhydride or contain carboxylic acid group or all or part of salt being neutralized into of sulfonic anionic monomer; The alkali that neutralization is used is ammoniacal liquor, sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood or sodium bicarbonate; Degree of neutralization in molar ratio percentage composition meter accounts for 50mol%-100mol%.
5. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, it is characterized in that, described cationic monomer is selected from one or more in following substances: acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamido oxypropyl trimethyl ammonium chloride, methacryloyl amido oxypropyl trimethyl ammonium chloride or diallyldimethylammonium chloride.
6. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, is characterized in that, the use total amount of described non-ionic monomer, anionic monomer and cationic monomer accounts for the 10%-60% of both sexes water-in-oil reversed-phase emulsion total mass; The mass ratio of described non-ionic monomer total amount and zwitterion monomer total amount is 1:19～19:1.
7. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, is characterized in that, described water quality stabilizer is sequestrant; The consumption of sequestrant is the 0.005%-0.1% of water quality.
8. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 7, is characterized in that, described sequestrant is disodium edta or diethylene triamine pentacetic acid (DTPA) five sodium-salt.
9. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 1, is characterized in that, described molecular weight regulator is the water-soluble substances with chain transfer; The consumption of molecular weight regulator is no more than 2% of the both sexes water-in-oil reversed-phase emulsion total mass preparing.
10. the preparation method of both sexes water-in-oil reversed-phase emulsion according to claim 9, is characterized in that: lower aliphatic alcohols, mercaptan, formate, methallylsulfonic acid sodium or urea that the described water-soluble substances with chain transfer is C1-C4.
The preparation method of 11. both sexes water-in-oil reversed-phase emulsions according to claim 1, is characterized in that, the saturated or unsaturated hydrocarbons that described varsol is C6-C30; The usage quantity of varsol is the 10%-50% of both sexes water-in-oil reversed-phase emulsion total mass.
The preparation method of 12. both sexes water-in-oil reversed-phase emulsions according to claim 1, is characterized in that, described emulsifying agent is nonionic emulsifying agent, and its hydrophile-lipophile balance value is 2.0-15.0; The consumption of emulsifying agent is the 1%-15% of both sexes water-in-oil reversed-phase emulsion total mass.
The preparation method of 13. both sexes water-in-oil reversed-phase emulsions according to claim 12, is characterized in that: described nonionic emulsifying agent is selected from one or more in following substances: sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, aliphatic alcohol polyethenoxy base ether, sorbyl alcohol glycidyl ester ether, polyoxyethylene carboxylate, alkylphenol-polyethenoxy base ether or aromatic series polyoxyethylene ether.
The preparation method of 14. both sexes water-in-oil reversed-phase emulsions according to claim 1, is characterized in that, described initiator is initiator, the peroxide initiator that contains azo group or the redox initiator being made up of Oxidizing and Reducing Agents; Initiator amount is the 0.001%-0.1% of both sexes water-in-oil reversed-phase emulsion total mass.
The preparation method of 15. both sexes water-in-oil reversed-phase emulsions according to claim 14, is characterized in that, the described initiator that contains azo group is azo di-isopropyl imidazoline salt hydrochlorate, azo diisobutyl amidine hydrochloride or Diisopropyl azodicarboxylate; Described peroxide initiator is hydrogen peroxide, dibenzoyl peroxide or tertbutyl peroxide; In the described redox initiator being made up of Oxidizing and Reducing Agents, oxygenant is selected from one or more in following substances: persulphate, bromate or superoxide; In the described redox initiator being made up of Oxidizing and Reducing Agents, reductive agent is selected from one or more in following substances: sulphite, lay particular stress on sulphite, thiosulphate, Fe
2+, Cu
+or organic amine.
The preparation method of 16. both sexes water-in-oil reversed-phase emulsions according to claim 14, it is characterized in that, described initiator is the redox initiator being made up of Oxidizing and Reducing Agents, when it uses, in water, first add described oxygenant, after mixing and emulsifying, add described reductive agent, the consumption of oxygenant and reductive agent is 1:2-2:1 again.
The preparation method of 17. both sexes water-in-oil reversed-phase emulsions according to claim 15, is characterized in that: described oxygenant is selected from one or more in following substances: Sodium Persulfate, ammonium persulphate, Potassium Persulphate, sodium bromate, potassium bromate, hydrogen peroxide, tertbutyl peroxide or dibenzoyl peroxide; Described reductive agent is selected from one or more in following substances: S-WAT, sodium bisulfite, Sodium Metabisulfite, Sulfothiorine, V-Brite B, iron protochloride, ferrous sulfate, cuprous chloride, triethylamine, trolamine or Tetramethyl Ethylene Diamine.
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| CN104071857A (en) * | 2014-07-17 | 2014-10-01 | 天津亿利科能源科技发展股份有限公司 | Preparation method for water clarifier for treating low-temperature thick-oil oily sewage in oilfield |
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