The preparation method and application of dry-powder putty sodium carboxymethylcellulose thickener rheology agent
Technical field
The present invention relates to a kind of thickener rheology agent, and in particular to a kind of preparation method of dry-powder putty thickener rheology agent and
Using.
Background technology
Dry-powder putty is one kind of building and ornament materials, and the repairing for building wall is levelling, due to easy to use, in recent years
To quickly grow.Dry-powder putty is mainly mixed by inorganic cementitious material, inorganic filler and other fine chemistry industry additives.Its
In, conventional inorganic cementitious material includes gypsum, cement, sierozem power etc., and general addition is 20 ~ 30%, play offer bond,
Improve the effect such as dry-powder putty surface strength;Conventional inorganic filler generally includes various stone flours, modified stone flour etc., accounts for whole dry
The 70 ~ 80% of powder putty, it is the main material of dry-powder putty filling;Conventional fine chemistry industry additive is mainly some polymer
Class additive, only accounting between 0.5 ~ 3.0% in dry-powder putty, but can substantially change the application property of product, assist to bond
Property, or improve some particular characteristics of dry-powder putty, it is the Core Feature material of putty.Sodium carboxymethylcellulose(CMC) it is
A kind of the most commonly used fine chemistry industry additive --- thickener rheology agent, its aqueous solution belong to pseudoplastic fluid in dry-powder putty, its
Viscosity reduces with the increase of shear stress, therefore can improve criticizing for dry-powder putty and scrape performance, while water conservation, anti-sag, and
With certain caking property.
The substitution value of general industry level sodium carboxymethylcellulose is mostly 0.75 ~ 0.95 in existing market.This substitution value
CMC product when being used for putty and batch scraping, viscosity is big, and feel is puckery, and not only the labor intensity of worker is big, and the metope after batch scraping is put down
Whole degree is poor.Therefore, that how to improve dry-powder putty criticizes the difficult point for scraping that performance is always work.
The content of the invention
To solve above mentioned problem existing for prior art, flowed it is an object of the invention to provide a kind of dry-powder putty with thickening
Become the preparation method and application of additive, the addition of the thickening rheologic additive can significantly improve batch the scraping property of dry-powder putty
Can, improve to criticize and scrape efficiency.
To achieve the above object, the technical solution adopted in the present invention is:
A kind of preparation method of dry-powder putty sodium carboxymethylcellulose thickener rheology agent, using fibrillation as raw material, including
Four pretreatment, alkalization, etherificate, post processing processes.
It is concretely comprised the following steps:
A, pre-process
Fibrillation is ground into it is cotton-shaped, it is stand-by;
The ethanol that the liquid caustic soda that mass fraction is 50% is 85% ~ 93% with volume fraction is mixed into basifier, basifier is cold
But it is stand-by to 18 ~ 30 DEG C;
The solid monoxone that mass fraction is 97.5% is dissolved in the ethanol solution that volume fraction is 89 ~ 92%, obtained
Mass fraction is 70 ~ 75% monoxone ethanol water, is cooled to 20 ~ 25 DEG C, stand-by;
B, alkalize
Cotton-shaped fibrillation is added and mediated in reactor, while sprays basifier;The addition time of cotton-shaped fibrillation be 15 ~
25 minutes, basifier spray time 20 ~ 30 minutes;Alkali alcohol stirs after spraying carries out quaternization for 30 ~ 40 minutes, and alkalization is anti-
15 ~ 25 DEG C of temperature should be controlled;
After the completion of alkalization, the monoxone ethanol water that mass fraction is 70 ~ 75% is uniformly sprayed to kneading reactor
In, spray time 20 ~ 40 minutes, 20 ~ 30 DEG C of control system temperature;After the completion of monoxone ethanol water spray, then uniformly add
Enter 5 ~ 30 mass parts acidic materials, then proceed to mixing 20 ~ 30 minutes, 25 ~ 30 DEG C of control system temperature;
C, it is etherified
Said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 75 ~ 80 DEG C of etherification reaction temperature, treats ethanol
After the completion of recovery, etherification reaction terminates;
D, post-process
Product carries out dries pulverizing after being etherified;Mixture enters dryer, and drying temperature is controlled at 110 ~ 120 DEG C, control
Material moisture < 10% after system drying, by crushing, batch mixing, sieving, splicing, pack and produce dry-powder putty carboxymethyl cellulose
Plain sodium thickener rheology agent product.
In the step A, the dosage of fibrillation is 100 mass parts;When preparing basifier, the dosage of liquid caustic soda is 90 ~ 100 matter
Measure part, the dosage of ethanol is 170 ~ 220 mass parts;When preparing monoxone ethanol water, the chloroacetic dosage of solid is 50 ~ 55
Mass parts, the dosage of ethanol is 20 ~ 30 mass parts;The liquid caustic soda is sodium hydroxide solution or potassium hydroxide solution.
In the step B, quaternization temperature is 20 ± 2 DEG C, and alkalization time is 60 ~ 70min;72 ~ 75% monoxone ethanol
The spray flux of the aqueous solution is 70 ~ 80 mass parts, and spray temperature control is at 25 ~ 30 DEG C;The acidic materials are acetic acid, hydrochloric acid, phosphorus
Acid, most preferably hydrophosphate, preferably hydrophosphate, sodium dihydrogen phosphate.
In the step C, the etherification reaction time is 60 ~ 120min.
In the step D, crush and use the vortex selection by winnowing grade grinder without sieve plate, crushing rear material moisture <
6%;Its size distribution is:
60 mesh |
0~0.1% |
60 ~ 80 mesh |
0.1~0.5% |
80 ~ 100 mesh |
0.5~1.0% |
100 ~ 200 mesh |
1.0~10.0% |
200 mesh and following |
85~95% |
The dry-powder putty with the consistency coefficient 9000 of 1.37% aqueous solution of sodium carboxymethylcellulose thickener rheology agent ~
12000mPa·Sn;Liquidity index n is 0.55 ~ 0.60.
Addition of the thickener rheology agent in dry-powder putty is 0.4 ~ 0.6%, preferably 0.5 ~ 0.55%.
The beneficial effects of the invention are as follows:
A kind of preparation method the invention provides dry-powder putty with sodium carboxymethylcellulose thickener rheology agent, reduces carboxylic
The substitution value of sodium carboxymethylcellulose pyce, it is set to be more suitable for the requirement of dry-powder putty.Product made from the inventive method, dissolving
Speed is fast, and viscosity, consistency coefficient and liquidity index are all very suitable for dry-powder putty use so that dry-powder putty batch is scraping process
Middle feel is brisk, not glutinous greasy, not sagging, effectively improves and batch scrapes performance, improves and batch scrapes efficiency, reduces the labor intensity of worker.
During the etherification reaction of the present invention, in addition to adding monoxone ethanol water as etherifying agent, also especially add
Enter acidic materials, acidic materials add can be excessive in neutralization system alkali, etherification reaction is gently carried out, help to improve
The alkalization effect of fiber, makes alkali be preferably minimized the damage capability of fiber, while improves the uniformity of etherification reaction, improves carboxylic first
The consistency coefficient and consistometric value of base cellulose.Acidic materials used in the present invention are acetic acid, hydrochloric acid, phosphoric acid, hydrophosphate, excellent
Elect hydrophosphate as, the dissociation constant of hydrophosphate is smaller, low to the destructive power of fiber, and the influence to etherification reaction is minimum.
Embodiment
The present invention is described in further detail below by specific embodiment, but embodiment is not the scope of the present invention
Limitation.
Unless otherwise specified, part described in the following example is mass parts.Raw materials used embodiment is commercially available production
Product.
Embodiment 1
A kind of dry-powder putty sodium carboxymethylcellulose thickener rheology agent, its preparation method are:
A, pre-process
100 parts of fibrillation are ground into cotton-shaped stand-by;
The liquid caustic soda that 95 parts of mass fractions are 50% and the ethanol that 185 parts of volume fractions are 89% are mixed into basifier, and it is cold
But it is stand-by to 25 DEG C;
The solid monoxone that 53 parts of mass fractions are 97.5% is dissolved in the ethanol solution that 23 parts of volume fractions are 92%,
The monoxone ethanol water that mass fraction is 70% is obtained, is cooled to 24 DEG C, it is stand-by;
B, alkalize
Cotton-shaped fibrillation is added and mediated in reactor, while sprays basifier;The addition time of cotton-shaped fibrillation is 20
Minute, basifier spray time 25 minutes;Alkali alcohol stirs after spraying carries out quaternization for 35 minutes, quaternization control temperature
18 ~ 21 DEG C of degree;
After the completion of alkalization, monoxone ethanol water is uniformly sprayed to and mediated in reactor, spray time 30 minutes, control
25 ~ 30 DEG C of system temperature processed;After the completion of monoxone ethanol water spray, then the sodium dihydrogen phosphate of 7.7 parts of quality is uniformly added into,
Then proceed to mixing 20 ~ 30 minutes, 25 ~ 28 DEG C of control system temperature;
C, it is etherified
Said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 ~ 80 DEG C of etherification reaction temperature, treats ethanol
After the completion of recovery, etherification reaction terminates;
D, post-process
Product carries out dries pulverizing after being etherified;Material enters dryer, and temperature control is at 110 ~ 120 DEG C, control drying
Material moisture is in < 10% afterwards, material by crushing, batch mixing, sieving, splicing, pack and produce dry-powder putty carboxymethyl cellulose
Plain sodium thickener rheology agent product.
Dry-powder putty sodium carboxymethylcellulose thickener rheology agent prepared by the present embodiment, its 1.37% aqueous solution it is thick
Spend coefficient 10800mPaSn, liquidity index 0.60, moisture 4.3%, its size distribution is:
60 mesh |
0.03% |
60 ~ 80 mesh |
0.2% |
80 ~ 100 mesh |
0.8% |
100 ~ 200 mesh |
5.6% |
200 mesh and following |
93.37% |
The present embodiment carboxymethyl cellulose thickener rheology agent is 0.55% in the optimum addition of dry-powder putty;After addition, do
Powder putty feel during batch scraping is brisk, not glutinous greasy, not sagging, and it is good batch to scrape performance, batch scrapes efficiency high.
Embodiment 2
A kind of dry-powder putty sodium carboxymethylcellulose thickener rheology agent, its preparation method are:
A, pre-process
100 parts of fibrillation are ground into cotton-shaped stand-by;
The liquid caustic soda that 92 parts of mass fractions are 50% and the ethanol that 200 parts of volume fractions are 89% are mixed into basifier, and it is cold
But it is stand-by to 25 DEG C;
The solid monoxone that 51 parts of mass fractions are 97.5% is dissolved in the ethanol solution that 21 parts of volume fractions are 92%,
The monoxone ethanol water solution that mass fraction is 70.8% is obtained, is cooled to 22 DEG C, it is stand-by;
B, alkalize
Cotton-shaped fibrillation is added and mediated in reactor, while sprays basifier;The addition time of cotton-shaped fibrillation is 20
Minute, basifier spray time 30 minutes;Alkali alcohol stirs after spraying carries out quaternization for 30 minutes, quaternization control temperature
18 ~ 21 DEG C of degree;
After the completion of alkalization, monoxone ethanol water is uniformly sprayed to and mediated in reactor, spray time 30 minutes, control
25 ~ 30 DEG C of system temperature processed;After the completion of monoxone ethanol water spray, then the sodium dihydrogen phosphate of 9 parts of quality is uniformly added into, so
After continue mixing 20 ~ 30 minutes, 25 ~ 28 DEG C of control system temperature;
C, it is etherified
Said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 ~ 80 DEG C of etherification reaction temperature, treats ethanol
After the completion of recovery, etherification reaction terminates;
D, post-process
Product carries out dries pulverizing after being etherified;Material enters dryer, and temperature control is at 110 ~ 120 DEG C, control drying
Material moisture is in < 10% afterwards, material by crushing, batch mixing, sieving, splicing, pack and produce dry-powder putty carboxymethyl cellulose
Plain sodium thickener rheology agent product.
Dry-powder putty sodium carboxymethylcellulose thickener rheology agent prepared by the present embodiment, its 1.37% aqueous solution it is thick
Spend coefficient 10000mPaSn, liquidity index 0.58, moisture 4.2%, its size distribution is:
60 mesh |
0.02% |
60 ~ 80 mesh |
0.1% |
80 ~ 100 mesh |
1.2% |
100 ~ 200 mesh |
6.3% |
200 mesh and following |
93.37% |
The present embodiment carboxymethyl cellulose thickener rheology agent is 0.50% in the optimum addition of dry-powder putty;After addition, do
Powder putty feel during batch scraping is brisk, not glutinous greasy, not sagging, and it is good batch to scrape performance, batch scrapes efficiency high.
Embodiment 3
A kind of dry-powder putty sodium carboxymethylcellulose thickener rheology agent, its preparation method are:
A, pre-process
100 parts of fibrillation are ground into cotton-shaped stand-by;
The liquid caustic soda that 90 parts of mass fractions are 50% and the ethanol that 200 parts of volume fractions are 89% are mixed into basifier, and it is cold
But it is stand-by to 25 DEG C;
The solid monoxone that 50 parts of mass fractions are 97.5% is dissolved in the ethanol solution that 22 parts of volume fractions are 92%,
The monoxone ethanol water that mass fraction is 69.5% is obtained, is cooled to 20 DEG C, it is stand-by;
B, alkalize
Cotton-shaped fibrillation is added and mediated in reactor, while sprays basifier;The addition time of cotton-shaped fibrillation is 20
Minute, basifier spray time 25 minutes;Alkali alcohol stirs after spraying carries out quaternization for 25 minutes, quaternization control temperature
18 ~ 21 DEG C of degree;
After the completion of alkalization, monoxone ethanol water is uniformly sprayed to and mediated in reactor, spray time 25 minutes, control
25 ~ 30 DEG C of system temperature processed;After the completion of monoxone ethanol water spray, then the sodium dihydrogen phosphate of 9 parts of quality is uniformly added into, so
After continue mixing 20 ~ 30 minutes, 25 ~ 28 DEG C of control system temperature;
C, it is etherified
Said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 ~ 80 DEG C of etherification reaction temperature, treats ethanol
After the completion of recovery, etherification reaction terminates;
D, post-process
Product carries out dries pulverizing after being etherified;Material enters dryer, and temperature control is at 110 ~ 120 DEG C, control drying
Material moisture is in < 10% afterwards, material by crushing, batch mixing, sieving, splicing, pack and produce dry-powder putty carboxymethyl cellulose
Plain sodium thickener rheology agent product.
Dry-powder putty sodium carboxymethylcellulose thickener rheology agent prepared by the present embodiment, its 1.37% aqueous solution it is thick
Spend coefficient 11000mPaSn, liquidity index 0.59, moisture 4.0%, its size distribution is:
60 mesh |
0.01% |
60 ~ 80 mesh |
0.5% |
80 ~ 100 mesh |
1.2 % |
100 ~ 200 mesh |
5.5% |
200 mesh and following |
92.79% |
The present embodiment carboxymethyl cellulose thickener rheology agent is 0.50% in the optimum addition of dry-powder putty;After addition, do
Powder putty feel during batch scraping is brisk, not glutinous greasy, not sagging, and it is good batch to scrape performance, batch scrapes efficiency high.
Comparative example 1
The preparation process of comparative example 1 and embodiment 1 is essentially identical, and it is differed only in:In step B, monoxone ethanol water
Sodium dihydrogen phosphate is not added with after the completion of solution spraying, is directly etherified.
Dry-powder putty sodium carboxymethylcellulose thickener rheology agent prepared by the present embodiment, its 1.37% aqueous solution it is thick
Spend coefficient 14000mPaSn, liquidity index 0.53, moisture 4.5%, its size distribution is:
60 mesh |
0.4% |
60 ~ 80 mesh |
1.2% |
80 ~ 100 mesh |
5.8% |
100 ~ 200 mesh |
15.5% |
200 mesh and following |
77.1% |
Comparative example 2
Using the carboxymethyl cellulose product as a comparison case 2 of commercially available substitution value 0.80, the denseness system of its 1.37% aqueous solution
Number is 7000mPaSn, liquidity index 0.75, moisture 7.5%, its size distribution is:
60 mesh |
0.8% |
60 ~ 80 mesh |
2.2% |
80 ~ 100 mesh |
6.8% |
100 ~ 200 mesh |
18.5% |
200 mesh and following |
71.7% |
Example 1 ~ 3, the product of comparative example 1 ~ 2 are added in dry-powder putty, are done to criticize and are scraped experiment.Specifically test situation is:
By powdered whiting:Organic binder bond:Thickener rheology agent=1:0.8%:0.5% ratio is mixed, and is added certain
The water of amount is stirred, and upper wall batch is scraped after standing dissolving certain time, intensity after detecting its workability and drying.Testing result
It is shown in Table 1.
Wall experiment conclusion on the powder of lacquer putty for use on of table 1
|
Dissolution time/minute |
Application property |
Intensity after drying |
Embodiment 1 |
12~13 |
Scratch accessible, smooth, feel is light |
It is qualified |
Embodiment 2 |
10~11 |
Scratch accessible, smooth, feel is brisk |
It is qualified |
Embodiment 3 |
9~10 |
Scratch accessible, smooth, feel is brisk |
It is qualified |
Comparative example 1 |
10~11 |
Obstacle is scratched, is had some setbacks, feel is slightly heavy |
It is qualified |
Comparative example 2 |
>20 |
Obstacle is scratched, viscous, feel is sunk |
It is qualified |
It is can be seen that by above-mentioned data compared with being added without the product of acidic materials when commercially available prod and alkalization, this hair
Bright product batch scrapes significant effect raising, moreover, dissolution time is short, blade coating is accessible, batch scraping efficiency greatly improves, worker's work
Intensity decreases.
Above-described embodiment is used for illustrating the present invention, rather than limits the invention, in the claims in the present invention
Protection domain in, to any modifications and changes for making of the present invention, both fall within protection scope of the present invention.