The dry-powder putty preparation method of sodium carboxymethyl cellulose thickener rheology agent and application
Technical field
The present invention relates to a kind of thickener rheology agent, be specifically related to preparation method and the application of a kind of dry-powder putty thickener rheology agent.
Background technology
Dry-powder putty is the one of building and ornament materials, and the repairing for building wall is levelling, and due to easy to use, development in recent years is rapid.Dry-powder putty is mainly mixed by inorganic cementitious material, inorganic filler and other fine chemistry industry additives.Wherein, conventional inorganic cementitious material includes Gypsum Fibrosum, cement, sierozem power etc., and general addition is 20 ~ 30%, plays offer bonding, improves the effects such as dry-powder putty surface strength;Conventional inorganic filler generally includes various stone powder, modified stone powder etc., accounts for the 70 ~ 80% of whole dry-powder putty, is the main material of dry-powder putty filling;Conventional fine chemistry industry additive is mainly some polymer class additives, only accounting between 0.5 ~ 3.0% in dry-powder putty, but can substantially change the application property of product, assist caking property, or improve some particular characteristic of dry-powder putty, be the Core Feature material of putty.Sodium carboxymethyl cellulose (CMC) is a kind of fine chemistry industry additive---thickener rheology agent the most commonly used in dry-powder putty, its aqueous solution belongs to pseudoplastic fluid, its viscosity reduces with the increase of shear stress, therefore can improve criticizing of dry-powder putty and scrape performance, water conservation, anti-sag simultaneously, and there is certain caking property.
In existing market, the substitution value of general industry level sodium carboxymethylcellulose is mostly 0.75 ~ 0.95.The CMC product of this substitution value is criticized for putty when scraping, and viscosity is big, and feel is puckery, and not only the labor intensity of workman is big, and it is poor to criticize the degree of plainness for wall surface after scraping.Therefore, batch scraping performance and being always up the difficult point of work of dry-powder putty how is improved.
Summary of the invention
For solving the problems referred to above that prior art exists, it is an object of the invention to provide the preparation method and application of a kind of dry-powder putty thickening rheologic additive, the addition of this thickening rheologic additive can significantly improve criticizing of dry-powder putty and scrape performance, improves to criticize and scrapes efficiency.
For achieving the above object, the technical solution adopted in the present invention is:
The preparation method of a kind of dry-powder putty sodium carboxymethyl cellulose thickener rheology agent, with fibril for raw material, including pretreatment, alkalization, etherificate, four operations of post processing.
It concretely comprises the following steps:
A, pretreatment
Fibril is ground into cotton-shaped, stand-by;
The liquid caustic soda that mass fraction is 50% is mixed into basifier with the ethanol that volume fraction is 85% ~ 93%, basifier is cooled to 18 ~ 30 DEG C, stand-by;
The solid monoxone that mass fraction is 97.5% is dissolved in the alcoholic solution that volume fraction is 89 ~ 92%, obtains the monoxone ethanol water that mass fraction is 70 ~ 75%, be cooled to 20 ~ 25 DEG C, stand-by;
B, alkalization
Cotton-shaped fibril is added and mediates in reactor, spray basifier simultaneously;The cotton-shaped fibriilar joining day is 15 ~ 25 minutes, basifier spray time 20 ~ 30 minutes;After alkali alcohol spray, stirring carries out quaternization in 30 ~ 40 minutes, and quaternization controls temperature 15 ~ 25 DEG C;
After having alkalized, uniformly it is sprayed to mediate in reactor by the monoxone ethanol water that mass fraction is 70 ~ 75%, spray time 20 ~ 40 minutes, controls system temperature 20 ~ 30 DEG C;After monoxone ethanol water has sprayed, then it is uniformly added into 5 ~ 30 mass parts acidic materials, then proceedes to mixing 20 ~ 30 minutes, control system temperature 25 ~ 30 DEG C;
C, etherificate
Being delivered in methyltertiarvbutyl ether reactor by said mixture and carry out etherification reaction, etherification reaction temperature 75 ~ 80 DEG C, after ethanol has reclaimed, etherification reaction terminates;
D, post processing
Undertaken product after etherificate drying and pulverize;Mixture enters dehydrator, dries temperature and controls at 110 ~ 120 DEG C, material moisture < 10% after controlling to dry, through pulverizing, batch mixing, sieve, namely splicing, packaging obtain dry-powder putty sodium carboxymethyl cellulose thickener rheology agent product.
In described step A, fibriilar consumption is 100 mass parts;Preparation basifier time, the consumption of liquid caustic soda be 90 ~ 100 mass parts, ethanol consumption be 170 ~ 220 mass parts;During preparation monoxone ethanol water, the chloroacetic consumption of solid is 50 ~ 55 mass parts, and the consumption of ethanol is 20 ~ 30 mass parts;Described liquid caustic soda is sodium hydroxide solution or potassium hydroxide solution.
In described step B, quaternization temperature is 20 ± 2 DEG C, and alkalization time is 60 ~ 70min;The spray flux of 72 ~ 75% monoxone ethanol waters is 70 ~ 80 mass parts, and spray temperature controls at 25 ~ 30 DEG C;Described acidic materials are acetic acid, hydrochloric acid, phosphoric acid, hydrophosphate, it is preferred to hydrophosphate, it is most preferred that for sodium dihydrogen phosphate.
In described step C, the etherification reaction time is 60 ~ 120min.
In described step D, pulverize and adopt the eddy current selecting crude drugs with winnower grade grinder without sieve plate, crushing rear material moisture < 6%;Its particle size distribution is:
60 orders |
0~0.1% |
60 ~ 80 orders |
0.1~0.5% |
80 ~ 100 orders |
0.5~1.0% |
100 ~ 200 orders |
1.0~10.0% |
200 orders and following |
85~95% |
Consistency coefficient 9000 ~ 12000mPa S of 1.37% aqueous solution of described dry-powder putty sodium carboxymethyl cellulose thickener rheology agentn;Liquidity index n is 0.55 ~ 0.60.
Described thickener rheology agent addition in dry-powder putty is 0.4 ~ 0.6%, it is preferred to 0.5 ~ 0.55%.
The invention has the beneficial effects as follows:
The preparation method that the invention provides a kind of dry-powder putty sodium carboxymethyl cellulose thickener rheology agent, reduces the substitution value of sodium carboxymethyl cellulose so that it is be more suitable for the instructions for use of dry-powder putty.The product that the inventive method prepares, dissolution velocity is fast, and viscosity, consistency coefficient and liquidity index are all very suitable for dry-powder putty and use, make dry-powder putty batch to scrape feel in process brisk, glutinous not greasy, not sagging, effectively improve and batch scrape performance, improve to criticize and scrape efficiency, reduce the labor intensity of workman.
In the etherification reaction process of the present invention, in addition to monoxone ethanol water as etherifying agent outside, also it is specifically added acidic materials, the addition of acidic materials can be excessive in neutralization system alkali, make etherification reaction gentleness carry out, contribute to improving the alkalization effect of fiber, make alkali that the damage capability of fiber to be preferably minimized, improve the uniformity of etherification reaction simultaneously, improve consistency coefficient and the consistometric value of carboxymethyl cellulose.Acidic materials used in the present invention are acetic acid, hydrochloric acid, phosphoric acid, hydrophosphate, it is preferred to hydrophosphate, and the ionization constant of hydrophosphate is less, and the destructive power of fiber is low, and the impact of etherification reaction is minimum.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, but embodiment is not the restriction of scope.
If no special instructions, described in the following example part is mass parts.Embodiment is raw materials used is commercially available prod.
Embodiment 1
A kind of dry-powder putty sodium carboxymethyl cellulose thickener rheology agent, its preparation method is:
A, pretreatment
100 parts of fibrils are ground into cotton-shaped stand-by;
The ethanol that liquid caustic soda that 95 parts of mass fractions are 50% and 185 parts of volume fractions are 89% is mixed into basifier, and is cooled to 25 DEG C, stand-by;
The solid monoxone that 53 parts of mass fractions are 97.5% is dissolved in the alcoholic solution that 23 parts of volume fractions are 92%, obtains the monoxone ethanol water that mass fraction is 70%, be cooled to 24 DEG C, stand-by;
B, alkalization
Cotton-shaped fibril is added and mediates in reactor, spray basifier simultaneously;The cotton-shaped fibriilar joining day is 20 minutes, basifier spray time 25 minutes;After alkali alcohol spray, stirring carries out quaternization in 35 minutes, and quaternization controls temperature 18 ~ 21 DEG C;
After having alkalized, uniformly it is sprayed to monoxone ethanol water mediate in reactor, spray time 30 minutes, controls system temperature 25 ~ 30 DEG C;After monoxone ethanol water has sprayed, then it is uniformly added into the sodium dihydrogen phosphate of 7.7 parts of quality, then proceedes to mixing 20 ~ 30 minutes, control system temperature 25 ~ 28 DEG C;
C, etherificate
Being delivered in methyltertiarvbutyl ether reactor by said mixture and carry out etherification reaction, etherification reaction temperature 78 ~ 80 DEG C, after ethanol has reclaimed, etherification reaction terminates;
D, post processing
Undertaken product after etherificate drying and pulverize;Material enters dehydrator, and temperature controls at 110 ~ 120 DEG C, and after controlling to dry, material moisture is at < 10%, material through pulverizing, batch mixing, sieve, namely splicing, packaging obtain dry-powder putty sodium carboxymethyl cellulose thickener rheology agent product.
Dry-powder putty prepared by the present embodiment sodium carboxymethyl cellulose thickener rheology agent, the consistency coefficient 10800mPa S of its 1.37% aqueous solutionn, liquidity index is 0.60, moisture 4.3%, and its particle size distribution is:
60 orders |
0.03% |
60 ~ 80 orders |
0.2% |
80 ~ 100 orders |
0.8% |
100 ~ 200 orders |
5.6% |
200 orders and following |
93.37% |
The present embodiment carboxymethyl cellulose thickener rheology agent is 0.55% at the optimum addition of dry-powder putty;After interpolation, dry-powder putty is batch to scrape feel in process brisk, and glutinous not greasy, not sagging, it is good batch to scrape performance, batch scrapes efficiency height.
Embodiment 2
A kind of dry-powder putty sodium carboxymethyl cellulose thickener rheology agent, its preparation method is:
A, pretreatment
100 parts of fibrils are ground into cotton-shaped stand-by;
The ethanol that liquid caustic soda that 92 parts of mass fractions are 50% and 200 parts of volume fractions are 89% is mixed into basifier, and is cooled to 25 DEG C, stand-by;
The solid monoxone that 51 parts of mass fractions are 97.5% is dissolved in the alcoholic solution that 21 parts of volume fractions are 92%, obtains the monoxone ethanol water solution that mass fraction is 70.8%, be cooled to 22 DEG C, stand-by;
B, alkalization
Cotton-shaped fibril is added and mediates in reactor, spray basifier simultaneously;The cotton-shaped fibriilar joining day is 20 minutes, basifier spray time 30 minutes;After alkali alcohol spray, stirring carries out quaternization in 30 minutes, and quaternization controls temperature 18 ~ 21 DEG C;
After having alkalized, uniformly it is sprayed to monoxone ethanol water mediate in reactor, spray time 30 minutes, controls system temperature 25 ~ 30 DEG C;After monoxone ethanol water has sprayed, then it is uniformly added into the sodium dihydrogen phosphate of 9 parts of quality, then proceedes to mixing 20 ~ 30 minutes, control system temperature 25 ~ 28 DEG C;
C, etherificate
Being delivered in methyltertiarvbutyl ether reactor by said mixture and carry out etherification reaction, etherification reaction temperature 78 ~ 80 DEG C, after ethanol has reclaimed, etherification reaction terminates;
D, post processing
Undertaken product after etherificate drying and pulverize;Material enters dehydrator, and temperature controls at 110 ~ 120 DEG C, and after controlling to dry, material moisture is at < 10%, material through pulverizing, batch mixing, sieve, namely splicing, packaging obtain dry-powder putty sodium carboxymethyl cellulose thickener rheology agent product.
Dry-powder putty prepared by the present embodiment sodium carboxymethyl cellulose thickener rheology agent, the consistency coefficient 10000mPa S of its 1.37% aqueous solutionn, liquidity index is 0.58, moisture 4.2%, and its particle size distribution is:
60 orders |
0.02% |
60 ~ 80 orders |
0.1% |
80 ~ 100 orders |
1.2% |
100 ~ 200 orders |
6.3% |
200 orders and following |
93.37% |
The present embodiment carboxymethyl cellulose thickener rheology agent is 0.50% at the optimum addition of dry-powder putty;After interpolation, dry-powder putty is batch to scrape feel in process brisk, and glutinous not greasy, not sagging, it is good batch to scrape performance, batch scrapes efficiency height.
Embodiment 3
A kind of dry-powder putty sodium carboxymethyl cellulose thickener rheology agent, its preparation method is:
A, pretreatment
100 parts of fibrils are ground into cotton-shaped stand-by;
The ethanol that liquid caustic soda that 90 parts of mass fractions are 50% and 200 parts of volume fractions are 89% is mixed into basifier, and is cooled to 25 DEG C, stand-by;
The solid monoxone that 50 parts of mass fractions are 97.5% is dissolved in the alcoholic solution that 22 parts of volume fractions are 92%, obtains the monoxone ethanol water that mass fraction is 69.5%, be cooled to 20 DEG C, stand-by;
B, alkalization
Cotton-shaped fibril is added and mediates in reactor, spray basifier simultaneously;The cotton-shaped fibriilar joining day is 20 minutes, basifier spray time 25 minutes;After alkali alcohol spray, stirring carries out quaternization in 25 minutes, and quaternization controls temperature 18 ~ 21 DEG C;
After having alkalized, uniformly it is sprayed to monoxone ethanol water mediate in reactor, spray time 25 minutes, controls system temperature 25 ~ 30 DEG C;After monoxone ethanol water has sprayed, then it is uniformly added into the sodium dihydrogen phosphate of 9 parts of quality, then proceedes to mixing 20 ~ 30 minutes, control system temperature 25 ~ 28 DEG C;
C, etherificate
Being delivered in methyltertiarvbutyl ether reactor by said mixture and carry out etherification reaction, etherification reaction temperature 78 ~ 80 DEG C, after ethanol has reclaimed, etherification reaction terminates;
D, post processing
Undertaken product after etherificate drying and pulverize;Material enters dehydrator, and temperature controls at 110 ~ 120 DEG C, and after controlling to dry, material moisture is at < 10%, material through pulverizing, batch mixing, sieve, namely splicing, packaging obtain dry-powder putty sodium carboxymethyl cellulose thickener rheology agent product.
Dry-powder putty prepared by the present embodiment sodium carboxymethyl cellulose thickener rheology agent, the consistency coefficient 11000mPa S of its 1.37% aqueous solutionn, liquidity index is 0.59, moisture 4.0%, and its particle size distribution is:
60 orders |
0.01% |
60 ~ 80 orders |
0.5% |
80 ~ 100 orders |
1.2 % |
100 ~ 200 orders |
5.5% |
200 orders and following |
92.79% |
The present embodiment carboxymethyl cellulose thickener rheology agent is 0.50% at the optimum addition of dry-powder putty;After interpolation, dry-powder putty is batch to scrape feel in process brisk, and glutinous not greasy, not sagging, it is good batch to scrape performance, batch scrapes efficiency height.
Comparative example 1
Comparative example 1 is essentially identical with the preparation process of embodiment 1, and it differs only in: in step B, and monoxone ethanol water is not added with sodium dihydrogen phosphate after having sprayed, and is made directly etherificate.
Dry-powder putty prepared by the present embodiment sodium carboxymethyl cellulose thickener rheology agent, the consistency coefficient 14000mPa S of its 1.37% aqueous solutionn, liquidity index is 0.53, moisture 4.5%, and its particle size distribution is:
60 orders |
0.4% |
60 ~ 80 orders |
1.2% |
80 ~ 100 orders |
5.8% |
100 ~ 200 orders |
15.5% |
200 orders and following |
77.1% |
Comparative example 2
Adopting the carboxymethyl cellulose product of commercially available substitution value 0.80 as a comparison case 2, the consistency coefficient of its 1.37% aqueous solution is 7000mPa Sn, liquidity index 0.75, moisture 7.5%, its particle size distribution is:
60 orders |
0.8% |
60 ~ 80 orders |
2.2% |
80 ~ 100 orders |
6.8% |
100 ~ 200 orders |
18.5% |
200 orders and following |
71.7% |
Example 1 ~ 3, comparative example 1 ~ 2 product add in dry-powder putty, do to criticize and scrape test.Concrete test situation is:
In ground calcium carbonate: organic binder bond: the ratio of thickener rheology agent=1:0.8%:0.5% mixes, adding a certain amount of water and stir, after standing dissolving certain time, upper wall is criticized and is scraped, and detects its workability and dried intensity.Testing result is in Table 1.
Wall experiment conclusion on table 1 powder of lacquer putty for use on
|
Dissolution time/minute |
Application property |
Dried intensity |
Embodiment 1 |
12~13 |
Blade coating is accessible, smooth and easy, and feel is light |
Qualified |
Embodiment 2 |
10~11 |
Blade coating is accessible, smooth and easy, and feel is brisk |
Qualified |
Embodiment 3 |
9~10 |
Blade coating is accessible, smooth and easy, and feel is brisk |
Qualified |
Comparative example 1 |
10~11 |
Blade coating obstacle, has some setbacks, and feel is slightly heavy |
Qualified |
Comparative example 2 |
>20 |
Blade coating obstacle, viscous, feel is sunk |
Qualified |
By above-mentioned data it can be seen that compared with being added without the product of acidic materials during with commercially available prod and alkalization, batch the scraping effect and significantly improve of product of the present invention, and, dissolution time is short, blade coating is accessible, batch scrapes efficiency and is greatly improved, and labor strength reduces.
Above-described embodiment is used for illustrating the present invention, rather than limits the invention, in the protection domain of the claims in the present invention, and any amendment that the present invention is made and change, both fall within protection scope of the present invention.