CN114478963A

CN114478963A - Synthesis of zeolite molecular sieve copolymer water-retaining agent for desert control

Info

Publication number: CN114478963A
Application number: CN202111623949.3A
Authority: CN
Inventors: 胡荣汉
Original assignee: Guangxi Jingdian Chemical New Material Co ltd
Current assignee: Guangxi Jingdian Chemical New Material Co ltd
Priority date: 2021-12-23
Filing date: 2021-12-23
Publication date: 2022-05-13

Abstract

The invention relates to synthesis of a zeolite molecular sieve copolymer water-retaining agent for desert control, and relates to the field of chemical synthesis. The invention discloses a synthesis process of a water-retaining agent for desert control, which comprises the following steps: firstly, adding acrylic acid into a reaction kettle, dropwise adding sodium hydroxide solution into the acrylic acid while stirring for neutralization, measuring an acid value to determine a reaction end point, and pumping the neutralized acrylic acid into a polymerization kettle; adding acrylamide and a cross-linking agent into a polymerization kettle, stirring until the acrylamide and the cross-linking agent are mutually dissolved, adding zeolite molecular sieve superfine powder, starting ultrasonic wave to strongly disperse, adding an initiator, heating to polymerize until the solution is completely converted into gel, and pressurizing and discharging; placing the product in a drying box, vacuumizing, dehydrating and drying at constant temperature; and crushing and sieving the dried substance by a crusher, and bagging and storing the powder.

Description

Synthesis of zeolite molecular sieve copolymer water-retaining agent for desert control

Technical Field

The invention relates to the field of chemical synthesis, in particular to synthesis of a zeolite molecular sieve copolymer water-retaining agent suitable for planting in agriculture, forestry and grass industries.

Background

The desert water-retaining agent is prepared from a phase-free powder material and a coupling agent in a weight ratio of 100: 0.5-25; the inorganic powder material is any one or any combination of calcium carbonate, magnesium carbonate, talcum powder, coal gangue, fly ash, diatomite or desulfurized gypsum; the coupling agent is titanate coupling agent, RCA modifier, aluminate coupling agent, phosphate coupling agent or any one or any combination thereof. The sand water-retaining agent prepared by using the inorganic powder material and the coupling agent has insufficient water retention capacity and no use and popularization value.

Inquiring patent publication No. CN1021812948, the water-retaining agent material for desert greening invented by the Yongji of the sinus, etc.: the material is produced by raw materials and auxiliary materials in certain parts by weight: acrylic acid, a neutralizer, a water-soluble catalyst, industrial purified water, a cross-linking agent, a stabilizer, superfine dehydration modified attapulgite, a dispersant and bentonite with the mesh number of 800-; the preparation method comprises the steps of mixing, neutralizing, stirring, polymerizing and drying the materials.

The invention uses attapulgite, bentonite and other materials to polymerize and crosslink with sodium polyacrylate, and the product has poor repeated use effect and can not meet the water retention requirement of arid desert.

Object of the Invention

Aiming at the defects in the prior art, the invention aims to provide the zeolite molecular sieve copolymer water-retaining agent which is acid-resistant, alkali-resistant, sunlight-resistant, bacterium-resistant, long in service life, capable of absorbing and dehydrating water circularly and has the water retaining capacity meeting the severe drought requirement of desert.

Technical scheme

The invention provides a synthesis process of a zeolite molecular sieve copolymer water-retaining agent for desert control.

The invention is realized by adopting the following technical scheme: the synthesis process is characterized in that the zeolite molecular sieve, acrylamide and sodium acrylate are subjected to copolymerization reaction under the action of an initiator and a cross-linking agent, and the product is dried, crushed and sieved to prepare the zeolite molecular sieve copolymer water-retaining agent.

Further, the invention also provides a preparation method of the zeolite molecular sieve copolymer water-retaining agent, which is characterized by comprising the following steps:

A. neutralizing: firstly, adding acrylic acid into a reaction kettle, then quantitatively dropwise adding 10-50% sodium hydroxide solution into the acrylic acid, stirring and neutralizing at normal temperature, and adding the acrylic acid into a polymerization reaction kettle after detecting that the neutralization acid value is qualified;

B. polymerization: adding acrylamide and a cross-linking agent into a polymerization reaction kettle according to a formula, and stirring for fully dissolving; then adding zeolite molecular sieve superfine powder, stirring and primarily mixing uniformly, then starting ultrasonic waves, strongly dispersing, adding an initiator, heating to carry out polymerization reaction until the solution is completely converted into gel, and pressurizing and discharging;

C. and (3) drying: mechanically treating the gel, placing the gel in a drying box, vacuumizing, drying at constant temperature and dehydrating.

D. Crushing: and (4) crushing the dehydrated massive solid, sieving, bagging and storing.

Wherein the zeolite molecular sieve is selected from one of 3A, 4A and 5A or a mixture thereof in any proportion.

The zeolite molecular sieve is 100-300 mesh molecular sieve superfine powder.

The cross-linking agent is one or more of N, N-methylene bisacrylamide, titanate, RCA modifier and aluminate;

the initiator is one of potassium persulfate and ammonium persulfate.

Description of the drawings:

FIG. 1 is a process flow diagram of a preparation method of a zeolite molecular sieve copolymer water retention agent, and the figure is a schematic flow diagram only for explaining the invention.

The invention is further illustrated with the aid of the accompanying drawings:

(1) neutralizing: acrylic acid enters a reaction kettle R1 through a vessel V1 through a line 1 and a line 3; sodium hydroxide solution with the concentration of 10-50% enters a reaction kettle R1 from V2 through a pipeline 2 and a pipeline 3; neutralization reaction was carried out in reaction vessel R1 to give a sodium acrylate solution.

(2) Polymerization: the reactant in the reaction kettle R1 enters a reaction kettle R2 through a line 4; acrylamide enters reactor R2 from vessel V3 through line 5; the ultrafine zeolite molecular sieve enters a reaction kettle R2 from a container V5 through a line 6; initiator from vessel V4 enters reactor R2 via line 7; heating the mixture in an oil bath in a jacket of R2 at 60-90 ℃ to carry out polymerization for 2-8 hours.

(3) And (3) drying: the materials are pumped out by a pump through a reaction kettle R2, extruded into strip-shaped slices, and then enter a dryer R3 through a pipeline 8, and are dried for 4-12 hours at a constant temperature of 60-90 ℃ under the vacuum of 0.02-0.09 MPa for dehydration.

(4) Crushing: and (3) feeding the dried material into a crusher R4 through a conveying line 9, crushing, sieving by a sieve of 100-300 meshes, and feeding into a storage tank V6 through a conveying line 10 for storage.

The invention has the following advantages:

(1) stable performance, acid and alkali resistance, sunlight resistance, temperature resistance, crushing strength and good antibacterial performance.

(2) The repeated suction and desorption times can reach more than 5000 times, the utilization efficiency is high, and the service life can reach 10 years.

(3) The water absorption capacity of the copolymer is more than 3-5 times of that of a single zeolite molecular sieve, water is slowly released in a water-deficient environment, and the planting survival rate of desert arid regions is effectively improved.

(4) The operation and use are convenient, and the product is only required to be mixed with the desert sand soil in proportion.

(5) The product is environment-friendly, has no toxicity and harm to soil, plants, animals, water and human bodies, and can not cause secondary pollution.

(6) The raw materials are widely and easily available, the cost is low, and the economic value and the market prospect are achieved.

The specific implementation mode is as follows:

example 1

The present invention will be described in further detail with reference to the following examples and the accompanying drawings.

In the reaction process shown in the attached figure 1, 10L of reactor R1 is made of 316L stainless steel and is provided with a speed-adjusting stirring device; the reaction kettle R2 is 25L, is made of 316L stainless steel, is provided with an ultrasonic oscillator and is heated by an oil bath jacket; the volume of the drying box R3 is 20L, the material is 316L stainless steel, and the electric heating constant temperature and vacuum device is adopted; r4 is a crusher with a vibrating screen, the material is 316L stainless steel, and the diameter of the vibrating screen is between 100 and 200 meshes.

Firstly adding 2700g of acrylic acid into a reaction kettle R1, starting a stirring device, dropwise adding 5850g of 30% sodium hydroxide solution into the acrylic acid at normal temperature, reacting for 30 minutes, detecting that the acid value is less than or equal to 20, and pumping into a reaction kettle R2 by a pump; 4500g of acrylamide and 150g of cross-linking agent are sequentially added into the reaction kettle R2 and stirred to be fully dissolved; then 7500g zeolite molecular sieve superfine powder (150 meshes) is added, an ultrasonic oscillator is started while stirring, the frequency is controlled at 50000HZ for dispersing for 25 minutes, 7.5g potassium persulfate is added, the temperature of a kettle interlayer oil bath is raised to 70 ℃ for reaction for 6 hours, the reaction is stopped when the product is totally gelatinous, and the temperature is reduced to 40 ℃; guiding out by a pressure pump, putting the mixture into a drying box R3 in a block shape, keeping the temperature at 80 ℃, and drying for 6 hours under the vacuum pressure of 0.05 MPa; taking out the dried solid, crushing by a crusher R4, sieving by a 150-mesh vibrating screen, and bagging and storing the sample.

Example 2

Adding 1800g of acrylic acid into a reaction kettle R1 in a metering manner, starting stirring, dropwise adding 3250g of 35% sodium hydroxide solution into the acrylic acid, reacting for 45 minutes at normal temperature, and pumping into a reaction kettle R2 by a pump; 3000g of acrylamide and 100g of cross-linking agent are sequentially added into a reaction kettle R2 and stirred to be fully dissolved; then adding 5000g of zeolite molecular sieve (150 meshes) powder, starting an ultrasonic oscillator while stirring, controlling the frequency of 45000HZ, dispersing for 40 minutes, adding 5g of potassium persulfate, heating in an oil bath in an interlayer to 90 ℃ for reaction for 4 hours, completely gelling the reactants, and stopping the reaction and cooling to 40 ℃; the pressure is led out by a pump, and the mixture is put into a drying box R3, the temperature is kept at 90 ℃, a vacuum pump is started, and the pressure is 0.05MPa and the time is 8.5 hours; taking out the dried solid, crushing by a crusher R4, sieving by a 200-mesh vibrating screen, and bagging and storing the sample.

Claims

1. The synthesis of zeolite molecular sieve copolymer water-retaining agent for desert control includes the following steps:

A. neutralizing: firstly, adding acrylic acid into a reaction kettle, quantitatively dropwise adding 10-50% sodium hydroxide solution into the acrylic acid, stirring and neutralizing for 10-55 minutes, measuring an acid value to determine that neutralization is completed (the acid value is less than or equal to 20), and adding the acrylic acid into a polymerization kettle by a pump;

B. polymerization: adding acrylamide and a cross-linking agent into a polymerization reaction kettle, and stirring for 10-30 minutes to fully dissolve the acrylamide and the cross-linking agent; then adding zeolite molecular sieve superfine powder, controlling the particle size of the molecular sieve to be between 100 and 300 meshes, stirring and carrying out ultrasonic strong dispersion for 10 to 60 minutes, adding an initiator, heating to 50 to 95 ℃ to carry out polymerization reaction for 2 to 8 hours until the solution is completely converted into gel, and pumping out the material under pressure;

C. and (3) drying: and (3) mechanically treating the reactant gel, placing the reactant gel in a drying box, vacuumizing for 0.02-0.09 MPa, keeping the temperature at 60-90 ℃ for 4-12 hours, and dehydrating and drying.

D. Crushing: and crushing the dried solid by a crusher, sieving by a sieve of 100-300 meshes, and bagging and storing the powder.

2. The process of claim 1, wherein: and (3) a neutralization process, wherein the neutralization is finished when the concentration of sodium hydroxide is between 10 and 50 percent and the acid value is less than or equal to 20.

3. The process of claim 1, wherein: the polymerization process is one of 3A, 4A and 5A or their mixture in any proportion.

4. The process of claim 1, wherein: the polymerization process comprises the steps of selecting 100-300-mesh molecular sieve superfine powder as a zeolite molecular sieve; the ultrasonic dispersion frequency is 30000-60000 HZ, and the dispersion time is controlled to be 10-60 minutes.

5. The process of claim 1, wherein: the polymerization process is carried out by selecting one or any two of N, N-methylene bisacrylamide, titanate, RCA modifier and aluminate as cross-linking agent; the initiator is one of potassium persulfate and ammonium persulfate.

6. The process of claim 1, wherein: the drying process requires vacuum of 0.02-0.09 MPa, temperature of 60-90 ℃ and dehydration time of 4-12 hours.