CN110330595A - A kind of preparation method of modified wood tar ceramic dispersants - Google Patents

A kind of preparation method of modified wood tar ceramic dispersants Download PDF

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CN110330595A
CN110330595A CN201910386049.8A CN201910386049A CN110330595A CN 110330595 A CN110330595 A CN 110330595A CN 201910386049 A CN201910386049 A CN 201910386049A CN 110330595 A CN110330595 A CN 110330595A
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wood tar
parts
modified wood
temperature
ceramic dispersants
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李碧云
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • C04B35/63404Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
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  • Structural Engineering (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)

Abstract

The present invention provides a kind of preparation method of modified wood tar ceramic dispersants, its step are as follows: (1) after wood tar, urea, 2- vinylphenol, alkaline conditioner and water being added into reaction kettle, heating is begun to warm up, when temperature rises to 85~100 DEG C, opens stirring;(2) formaldehyde is slowly added dropwise, time for adding was controlled at 1~3 hour, temperature control is at 85~125 DEG C when dropwise addition, lignosulfonates, unsaturated carboxylic acid anhydrides are added after being added dropwise, then start that the initiator solution that mass percent concentration is 1~10% is added dropwise, this initiator solution is formulated by the water of the initiator and surplus, and time for adding control temperature at 0.5~3 hour, dropwise addition is controlled at 85~125 DEG C;(3) cooling discharge is after keeping the temperature 0.5~3 hour after adding to get the modified wood tar ceramic dispersants.

Description

A kind of preparation method of modified wood tar ceramic dispersants
The present invention is number of patent application: 201611010561.5, patent application day are as follows: on November 17th, 2016, proprietary term Referred to as: a kind of divisional application of modified wood tar ceramic dispersants and preparation method thereof.
Technical field
The present invention relates to ceramic dispersants technical field, in particular to a kind of preparation side of modified wood tar ceramic dispersants Method.
Background technique
Ceramic dispersants also known as ceramics liquefacient, degumming agent, water-reducing agent and diluent etc., one as ceramic additive Kind, major function is to destroy the flocculent structure of ceramic slurry particle, has slurry still in the lower situation of moisture content Preferable dispersibility and lower viscosity.Under the premise of guaranteeing mud proper flow and viscosity, containing for mud is reduced to the greatest extent Water rate is most important energy-saving means.The excellent dispersing agent of service performance can reduce the production of ceramics in Production of Ceramics Cost improves product quality, develops Production of Ceramics industry towards high efficiency, the direction that high-quality and low energy consumption.
Currently, the common dispersing agent of China ceramic industry has: waterglass, sodium phosphate, sodium tripolyphosphate, sodium pyrophosphate, six Sodium metaphosphate, sodium carbonate, sodium citrate, sodium humate, lignosulfite etc..These dispersing agents there are dispergation narrow range, Easily solidification, bad adaptability and the disadvantages of there are side effects in short time.A small number of Ceramics Enterprises are using organic dispersing agent and inorganic point Powder is used in combination, although certain effect can be played, the dispersing agent of exploitation does not have versatility, is not applied for various Different clay mineral raw materials, thus be difficult to promote the use of.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of preparations of modified wood tar ceramic dispersants Method, is had versatile using dispersing agent made from modification wood tar ceramic dispersants preparation method of the invention, dosage is small, Effect good advantage can make ceramic mud in the case where water content is reduced as far as possible, and reach the mobility of requirement after use 's.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of modified wood tar ceramic dispersants, is achieved by the steps of:
(1) it after wood tar, urea, 2- vinylphenol, alkaline conditioner and the part water being added into reaction kettle, opens Beginning heat temperature raising opens stirring when temperature rises to 85~100 DEG C;
(2) formaldehyde is slowly added dropwise, time for adding control temperature control at 1~3 hour, dropwise addition is added dropwise at 85~125 DEG C After be added lignosulfonates, unsaturated carboxylic acid anhydrides, then start be added dropwise mass percent concentration be 1~10% initiation Agent solution, this initiator solution are formulated by the water of the initiator and surplus, and time for adding was controlled at 0.5~3 hour, drop Added-time temperature is controlled at 85~125 DEG C;
(3) cooling discharge is after keeping the temperature 0.5~3 hour after adding to get the modified wood tar ceramic dispersants;
The alkaline conditioner be sodium hydroxide, potassium hydroxide, sodium carbonate, in potassium carbonate any one or it is two or more With the mixed mixture of any ratio.
The lignosulfonates are sodium lignin sulfonate, potassium lignosulfonate, any one in ammonium lignosulphonate Or it is two or more with the mixed mixture of any ratio.
The unsaturated carboxylic acid anhydrides be acrylic anhydride, methacrylic anhydride, any one or two kinds in maleic anhydride with On with the mixed mixture of any ratio.
The initiator be sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate in any one or it is two or more arbitrarily to compare Mixed mixture.
A kind of modified wood tar ceramic dispersants are mainly made of the raw material components that following portions by weight matches:
Compared with prior art, the present invention has following remarkable result:
1, modified wood tar ceramic dispersants prepared by the present invention are containing the functional groups such as carboxyl, sulfonic group, in additive amount and When other conditions are identical, relative to other ceramic dispersants, there is good mobility and viscosity, reached energy-saving mesh , while there is apparent reinforcing effect to biscuit of ceramics.
2, modified wood tar ceramic dispersants simple production process prepared by the present invention, mild condition, production process charging, Condition is all easy to control, it is easy to accomplish industrialized production.
Specific embodiment
The present invention is further elaborated on reference to embodiments.
A kind of modified wood tar ceramic dispersants of the invention are made of the raw material components that following portions by weight matches:
The alkaline conditioner be sodium hydroxide, potassium hydroxide, sodium carbonate, in potassium carbonate any one or it is two or more With the mixed mixture of any ratio.
The lignosulfonates are sodium lignin sulfonate, potassium lignosulfonate, any one in ammonium lignosulphonate Or it is two or more with the mixed mixture of any ratio.
The unsaturated carboxylic acid anhydrides be acrylic anhydride, methacrylic anhydride, any one or two kinds in maleic anhydride with On with the mixed mixture of any ratio.
The initiator is one or more of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate with any ratio mixing Mixture.
A kind of preparation method of modified wood tar ceramic dispersants, is achieved by the steps of:
(1) it after wood tar, urea, 2- vinylphenol, alkaline conditioner and the part water being added into reaction kettle, opens Beginning heat temperature raising opens stirring when temperature rises to 85~100 DEG C;
(2) formaldehyde is slowly added dropwise, time for adding control temperature control at 1~3 hour, dropwise addition is added dropwise at 85~125 DEG C After be added lignosulfonates, unsaturated carboxylic acid anhydrides, then start be added dropwise mass percent concentration be 1~10% initiation Agent solution, this initiator solution are formulated by the water of the initiator and surplus, and time for adding was controlled at 0.5~3 hour, drop Added-time temperature is controlled at 85~125 DEG C;
(3) cooling discharge is after keeping the temperature 0.5~3 hour after adding to get the modified wood tar ceramic dispersants.
With specific embodiment, the present invention is described in detail below, but the present invention is not limited only to this.
Embodiment one
A kind of modified wood tar ceramic dispersants are made of the raw material components that following portions by weight matches:
Preparation method is achieved by the steps of:
(1) into reaction kettle be added 12 parts of wood tar, 3 parts of urea, 1.5 parts of 2- vinylphenols, 4 parts of sodium hydroxides and After 56.5 parts of water, heating is begun to warm up, when temperature rises to 90 DEG C, opens stirring;
(2) 3 parts of formaldehyde are slowly added dropwise, time for adding control temperature control at 1.5 hours, dropwise addition is dripped at 95 DEG C 7 parts of sodium lignin sulfonates, 3 parts of acrylic anhydrides are added after finishing, then start that the sodium peroxydisulfate that mass percent concentration is 3% is added dropwise Solution, this sodium peroxydisulfate solution are formulated by 0.3 part of sodium peroxydisulfate and 9.7 parts of water, and time for adding control is small 1.5 When, temperature control is at 98 DEG C when dropwise addition;
(3) cooling discharge is after keeping the temperature 1.5 hours after adding to get the modified wood tar ceramic dispersants.
Embodiment two
A kind of modified wood tar ceramic dispersants are made of the raw material components that following portions by weight matches:
Preparation method is achieved by the steps of:
(1) 14 parts of wood tar of addition, 5 parts of urea, 2 parts of 2- vinylphenols, 3 parts of sodium hydroxides and 50 parts into reaction kettle After water, heating is begun to warm up, when temperature rises to 87 DEG C, opens stirring;
(2) 3 parts of formaldehyde are slowly added dropwise, time for adding control temperature control at 2 hours, dropwise addition is added dropwise at 105 DEG C 8 parts of sodium lignin sulfonates, 5 parts of acrylic anhydrides are added afterwards, it is molten then to start the sodium peroxydisulfate that dropwise addition mass percent concentration is 5% Liquid, this sodium peroxydisulfate solution are formulated by 0.5 part of sodium peroxydisulfate and 9.5 parts of water, and time for adding is controlled at 2 hours, dropwise addition Temperature is controlled at 110 DEG C;
(3) cooling discharge is after keeping the temperature 2.5 hours after adding to get the modified wood tar ceramic dispersants.
Embodiment three
A kind of modified wood tar ceramic dispersants are made of the raw material components that following portions by weight matches:
Preparation method is achieved by the steps of:
(1) into reaction kettle be added 16 parts of wood tar, 6 parts of urea, 2.5 parts of 2- vinylphenols, 3 parts of alkaline conditioners and After 41.5 parts of water, heating is begun to warm up, when temperature rises to 90 DEG C, opens stirring;
(2) 5 parts of formaldehyde are slowly added dropwise, time for adding control temperature control at 2.5 hours, dropwise addition is dripped at 115 DEG C 9 parts of potassium lignosulfonates, 7 parts of methacrylic anhydrides are added after finishing, then start that the over cure that mass percent concentration is 7% is added dropwise Sour potassium solution, this potassium persulfate solution are formulated by 0.7 part of potassium peroxydisulfate and 9.3 parts of water, and time for adding control is small 2.5 When, temperature control is at 120 DEG C when dropwise addition;
(3) cooling discharge is after keeping the temperature 2 hours after adding to get the modified wood tar ceramic dispersants.
Example IV
A kind of modified wood tar ceramic dispersants are made of the raw material components that following portions by weight matches:
Preparation method is achieved by the steps of:
(1) 18 parts of wood tar of addition, 7 parts of urea, 3 parts of 2- vinylphenols, 2 parts of potassium hydroxide and 40 parts into reaction kettle After water, heating is begun to warm up, when temperature rises to 98 DEG C, opens stirring;
(2) 5 parts of formaldehyde are slowly added dropwise, time for adding control temperature control at 2.5 hours, dropwise addition is dripped at 105 DEG C 7 parts of ammonium lignosulphonates, 8 parts of methacrylic anhydrides are added after finishing, then start that the over cure that mass percent concentration is 9% is added dropwise Sour potassium solution, this potassium persulfate solution are formulated by 0.9 part of potassium peroxydisulfate and 9.1 parts of water, and time for adding control is small 2.5 When, temperature control is at 112 DEG C when dropwise addition;
(3) cooling discharge is after keeping the temperature 2.5 hours after adding to get the modified wood tar ceramic dispersants.
Embodiment five
A kind of modified wood tar ceramic dispersants are made of the raw material components that following portions by weight matches:
Wherein:
Lignosulfonates use the mixture of sodium lignin sulfonate and potassium lignosulfonate, and sodium lignin sulfonate and wood The amount ratio of quality potassium sulfonate is 1:4, that is, the dosage of sodium lignin sulfonate and potassium lignosulfonate is respectively 1 part and 4 parts.
Preparation method is achieved by the steps of:
(1) 20 parts of wood tar, 7 parts of urea, 3.5 parts of 2- vinylphenols, 2 parts of sodium carbonate and 27.5 are added into reaction kettle After part water, heating is begun to warm up, when temperature rises to 97 DEG C, opens stirring;
(2) 7 parts of formaldehyde are slowly added dropwise, time for adding control temperature control at 2 hours, dropwise addition is added dropwise at 117 DEG C 1 part of sodium lignin sulfonate, 4 parts of potassium lignosulfonates, 8 parts of maleic anhydrides are added afterwards, then starts that mass percent concentration is added dropwise For 5% ammonium persulfate solution, this ammonium persulfate solution is formulated by 1 part of ammonium persulfate and 19 parts of water, time for adding control At 2.5 hours, dropwise addition, temperature control was at 120 DEG C;
(3) cooling discharge is after keeping the temperature 1.5 hours after adding to get the modified wood tar ceramic dispersants.
Embodiment six
A kind of modified wood tar ceramic dispersants are made of the raw material components that following portions by weight matches:
Wherein:
Unsaturated carboxylic acid anhydrides use the mixture of acrylic anhydride and methacrylic anhydride, and acrylic anhydride and methacrylic acid The amount ratio of acid anhydride is 1:2, that is, the dosage of acrylic anhydride and methacrylic anhydride is respectively 3 parts and 6 parts.
Initiator uses the mixture of sodium peroxydisulfate and potassium peroxydisulfate, and the amount ratio of sodium peroxydisulfate and potassium peroxydisulfate is 1: 1, that is, the dosage of sodium peroxydisulfate and potassium peroxydisulfate is respectively 0.75 part.
Preparation method is achieved by the steps of:
(1) 23 parts of wood tar, 8 parts of urea, 4 parts of 2- vinylphenols, 1.5 parts of potassium carbonate and 22.5 are added into reaction kettle After part water, heating is begun to warm up, when temperature rises to 95 DEG C, opens stirring;
(2) 9 parts of formaldehyde are slowly added dropwise, time for adding control temperature control at 2.5 hours, dropwise addition is dripped at 113 DEG C 3 parts of ammonium lignosulphonates, 3 parts of acrylic anhydrides, 6 parts of methacrylic anhydrides are added after finishing, it is dense then to start dropwise addition mass percent The initiator solution that degree is 7.5%, this initiator solution is by 0.75 part of sodium peroxydisulfate and 0.75 part of potassium peroxydisulfate and 18.5 parts of water It is formulated, time for adding control temperature at 2 hours, dropwise addition is controlled at 115 DEG C;
(3) cooling discharge is after keeping the temperature 2.5 hours after adding to get the modified wood tar ceramic dispersants.
The following are the performance comparison numbers for using modification wood tar ceramic dispersants and commercially available ceramic dispersants of the invention According to.Ceramic batch composition (wt%) is shown in Table 1.
1 ceramic batch of table composition
Clay Kaolin Feldspar Silica flour
40% 15% 30% 15%
The modification wood tar ceramic dispersants of 2 embodiment of the present invention one~six of table preparation and commercially available ceramic dispersants performance Contrast table
Remarks: 1, comparative sample is commercially available ceramic dispersants, is made by sodium tripolyphosphate and waterglass 5:2 in mass ratio Mixture;
2, the delivery time of ceramic slurry is using -4 glasss of measurements of painting, with 100 milliliters of slurries required times of outflow come table Show;
3, the test of green compact flexural strength is referring to the 4th part national standard GBT3810.4-2006: the modulus of rupture and breakdown strength Measurement.
The foregoing descriptions are merely the embodiment using this origination techniques content, any those skilled in the art use this wound Make done modifications and changes, all belong to the scope of the patents of this creation opinion, and is not limited to those disclosed embodiments.

Claims (2)

1. a kind of preparation method of modified wood tar ceramic dispersants, it is characterised in that: be achieved by the steps of:
(1) after wood tar, urea, 2- vinylphenol, alkaline conditioner and water being added into reaction kettle, heating is begun to warm up, When temperature rises to 85~100 DEG C, stirring is opened;
(2) formaldehyde is slowly added dropwise, time for adding control temperature control at 1~3 hour, dropwise addition is added dropwise at 85~125 DEG C Lignosulfonates, unsaturated carboxylic acid anhydrides are added afterwards, it is molten then to start the initiator that dropwise addition mass percent concentration is 1~10% Liquid, this initiator solution are formulated by the water of the initiator and surplus, and time for adding is controlled at 0.5~3 hour, dropwise addition Temperature is controlled at 85~125 DEG C;
(3) cooling discharge is after keeping the temperature 0.5~3 hour after adding to get the modified wood tar ceramic dispersants;
The alkaline conditioner be sodium hydroxide, potassium hydroxide, sodium carbonate, in potassium carbonate any one or it is two or more to appoint Meaning is than mixed mixture;
The lignosulfonates be sodium lignin sulfonate, potassium lignosulfonate, in ammonium lignosulphonate any one or two Kind or more with the mixed mixture of any ratio;
The unsaturated carboxylic acid anhydrides be acrylic anhydride, methacrylic anhydride, in maleic anhydride any one or it is two or more with The mixed mixture of any ratio;
The initiator be sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate in any one or it is two or more with it is any than mixing Mixture.
2. a kind of modified wood tar ceramic dispersants, it is characterised in that: the raw material components system mainly matched by following portions by weight At:
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CN110330595A (en) * 2016-11-17 2019-10-15 李碧云 A kind of preparation method of modified wood tar ceramic dispersants
CN108675801A (en) * 2018-06-17 2018-10-19 刘玉清 A kind of polymer ceramic liquefacient and preparation method thereof

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