Amphoteric rosin air-entraining agent and preparation method thereof

Through the oxidation reaction of modified rosin acid and modified A, combined with modified B and solvent, an amphoteric rosin induction agent with good surfactivity and acid-base salt resistance was prepared, which solved the problem of poor stability and foaming performance of rosin induction agents, and achieved better salt resistance, foaming ability and foaming stability performance.

CN117326969BActive Publication Date: 2025-03-21SHIJIAZHUANG CHANGAN YUCAI BUILDING MATERIALS +1
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Patent Information

Application Number
CN202311276255.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-30
Publication Date
2025-03-21
Estimated Expiration
2043-09-30

AI Technical Summary

Technical Problem

After being dissolved in water, the existing rosin gas induction agents are prone to complex with calcium and magnesium ions and precipitate, resulting in poor gas induction effect and poor stability and foaming performance.

Method used

By oxidizing the rosin acid and modified A under NaF catalyzing, an ultra-long chain amphoteric rosin induction agent is generated, and combined with modified B and solvent through subsequent reactions to form a final product with good surfactivity and acid-base salt resistance.

Benefits of technology

An amphoteric rosin initiator with good surfactivity and acid-base salt resistance in a wide pH range was achieved, which significantly improved its salt resistance, foaming ability and foaming stability, and solved the problem of poor stability and foaming performance of rosin initiator.

✦ Generated by Eureka AI based on patent content.

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Abstract

A kind of amphoteric rosin air-entraining agent and its preparation method, the present invention provides the structural formula of the amphoteric rosin air-entraining agent. The preparation method of the amphoteric rosin air-entraining agent comprises the following process steps: adding rosin acid and modifier A into a reactor, using NaF as a catalyst and aluminum oxide as a water absorbent, stirring and reacting at 150-170°C for 8-15h, adding acetone after the obtained material is cooled, stirring, filtering and drying to obtain a solid intermediate product; adding the intermediate product, modifier B and solvent into a reactor, reacting at 75-85°C for 8-15h, distilling off the solvent by reduced pressure after the reaction is completed, adding ethyl acetate, stirring, filtering and drying to obtain the final product, which is the amphoteric rosin air-entraining agent. The present invention has good air entraining performance and gas stabilizing performance, and has better salt resistance, foaming ability and foam stabilizing performance than the existing rosin air-entraining agent, thereby solving the problems of poor stability and poor foaming performance of the rosin air-entraining agent.
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Description

Technical Field

[0001] The invention relates to an air entraining agent for concrete, in particular to an amphoteric rosin air entraining agent and also relates to a preparation method of the amphoteric rosin air entraining agent. Background Art

[0002] Freeze-thaw damage to concrete causes premature cracking of concrete, which seriously damages the service life of concrete and becomes one of the main reasons affecting the durability of concrete. Adding air-entraining agent is one of the most widely used technical approaches, which can improve the frost resistance of concrete and improve the durability of concrete. In addition, introducing bubbles into fresh concrete can also improve the working performance of concrete and reduce the risk of concrete segregation and bleeding. Rosin air-entraining agent is the most studied and earliest applied air-entraining agent. It has a simple synthesis process and abundant raw materials. However, due to the presence of carboxyl groups, rosin air-entraining agent is easy to complex with calcium and magnesium ions after being dissolved in tap water, and precipitates, which greatly affects its air-entraining effect.

[0003] Related patent documents: CN110104986A discloses a method for preparing a novel composite concrete air entraining agent, which comprises: 5%-15% dodecyl dimethamine oxide, 5%-15% ethoxylated alkyl sodium sulfate, 5%-10% sodium rosin acid, 5%-15% coconut oil diethanolamide, and the balance is water. CN101898880A discloses an air entraining agent for concrete mixed with fly ash and a method for preparing the same, firstly adding water into a mixer, then adding rosin acid or rosin acid salt, alkyl sulfonate, alkylphenol polyoxyethylene ether, and higher fatty alcohol sulfate into the mixer in sequence, stirring and dissolving for 1-2 hours, to obtain an air entraining agent for concrete mixed with fly ash.

[0004] The above technologies do not provide specific guidance on how to make the amphoteric rosin air-entraining agent have good air-entraining and air-stabilizing properties and have better salt resistance, foaming ability and foam-stabilizing properties than the rosin air-entraining agent. Summary of the invention

[0005] The technical problem to be solved by the present invention is to provide an amphoteric rosin air-entraining agent, which has good air-entraining performance and air-stabilizing performance, and has better salt resistance, foaming ability and foam-stabilizing performance than the existing rosin air-entraining agent, thereby solving the problem of poor stability and poor foaming performance of the rosin air-entraining agent.

[0006] Therefore, another technical problem to be solved by the present invention is to provide a method for preparing the above-mentioned amphoteric rosin air-entraining agent.

[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:

[0008] An amphoteric rosin air-entraining agent, characterized in that the structural formula of the amphoteric rosin air-entraining agent is as follows:

[0009]

[0010] Wherein, R is a straight chain alkane of 2 to 4 carbon atoms.

[0011] The preparation method of the amphoteric rosin air-entraining agent comprises the following process steps: ① adding rosin acid and modified substance A into a reactor (reactor), using NaF as a catalyst and aluminum oxide as a water absorbent, stirring and reacting at 150-170°C for 8-15h, adding acetone to the obtained material after cooling, stirring, filtering and drying to obtain a solid intermediate product; ② adding the intermediate product, modified substance B and solvent into a reactor, reacting at 75-85°C for 8-15h, distilling off the solvent under reduced pressure after the reaction is completed, adding ethyl acetate, stirring, filtering and drying to obtain the final product, which is the amphoteric rosin air-entraining agent.

[0012] The above-mentioned modified substance A is one of N,N-dimethyl-1,3-ethylenediamine, N,N-dimethyl-1,3-propylenediamine, and N,N-dimethyl-1,3-butylenediamine; the mass ratio of rosin acid to modified substance A is 1:0.4-0.7, and the mass ratio of rosin acid, sodium fluoride, aluminum oxide, and acetone is 1:(0.02-0.1):(0.02-0.1):(5-8); the above-mentioned modified substance B is one of sodium chloroacetate and sodium bromoacetate; the mass ratio of the intermediate product, modified substance B, solvent, and ethyl acetate is 1:(0.4-0.8):(3-7):(3-7).

[0013] In the above technical scheme, a preferred technical scheme may be: the solvent is one or a combination of two raw materials selected from methanol, ethanol, isopropanol, and water (the ratio of the combination may be arbitrary).

[0014] In the above technical scheme, the preferred technical scheme can also be: the preparation method of the amphoteric rosin air-entraining agent comprises the following process steps: ① 30g of rosin acid and 13.5g of modified substance A, namely N,N-dimethyl-1,3-propylenediamine, are added into a reactor, and 0.6g of NaF is used as a catalyst, 1g of aluminum oxide is used as a water absorbent, and the mixture is stirred and reacted at 155°C for 9h. After the obtained material is cooled, 150g of acetone is added, and the mixture is stirred, filtered and dried to obtain a solid intermediate product; ② 32g of the intermediate product, 20g of the modified substance B, and a solvent are added to a reactor, and the mixture is reacted at 75°C for 10h. The modified substance B is sodium chloroacetate, and the solvent is a combination of 119mL of methanol (about 94.2g) and 10g of water. After the reaction is completed, the solvent is distilled off under reduced pressure, 130g of ethyl acetate is added, and the mixture is stirred, filtered and dried to obtain the final product, which is an amphoteric rosin air-entraining agent; the mass ratio of the above-mentioned rosin acid to the modified substance A is 1:0.45, and the mass ratio of the rosin acid, sodium fluoride, aluminum oxide, and acetone is 1:0.02:0.033:5; the mass ratio of the above-mentioned intermediate product, the modified substance B, the solvent, and ethyl acetate is 1:0.625:3.26:4.06.

[0015] In the above technical scheme, the preferred technical scheme can also be: the preparation method of the amphoteric rosin air-entraining agent comprises the following process steps: ① 30g of rosin acid and 16g of modified substance A, namely N,N-dimethyl-1,3-propylenediamine, are added to a reactor, 1.8g of NaF is used as a catalyst, 2.6g of aluminum oxide is used as a water absorbent, and the reaction is stirred at 165°C for 10h, and 170g of acetone is added to the obtained material after cooling, and a solid intermediate product is obtained after stirring, filtering and drying; ② 38g of the intermediate product, 23g of modified substance B, and a solvent are added to a reactor, and the reaction is carried out at 79°C for 12h, wherein the modified substance B is sodium chloroacetate, and the solvent is a combination of 150mL of ethanol (about 118.35g) and 30mL of water. After the reaction is completed, The solvent was distilled off under reduced pressure, 210 mL of ethyl acetate (about 189.42 g) was added, stirred, filtered and dried to obtain the final product, which was an amphoteric rosin air-entraining agent; the mass ratio of the above-mentioned rosin acid to the modifier A was 1:0.533, and the mass ratio of rosin acid, sodium fluoride, aluminum oxide and acetone was 1:0.06:0.087:5.67; the mass ratio of the above-mentioned intermediate product, modifier B, solvent and ethyl acetate was 1:0.61:3.9:4.98.

[0016] Among the above technical solutions, the preferred technical solutions may also be Example 3, Example 4, and Example 5 of the present application.

[0017] The present invention obtains a super-long-chain amphoteric rosin air-entraining agent by modifying rosin acid, so that the agent has good surface activity in a wide pH range, high acid, alkali and salt resistance, and low critical micelle concentration, thereby synthesizing an air-entraining agent with good foaming property and good foam stabilization performance. See the experimental part of the present invention: the air-entraining and air-stabilization performance of the present invention are good, and the agent has better salt resistance, foaming ability and foam stabilization performance than the existing rosin air-entraining agent, thereby solving the problem of poor stability and poor foaming performance of the rosin air-entraining agent.

[0018] The method of using the present invention can be carried out by adding it when mixing concrete or by compounding it with concrete admixtures. The dosage (addition amount) of the present invention is the total mass of the cementitious material in the concrete. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described in combination with the embodiments below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of them. Based on the embodiments in the invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] Example 6: The structural formula of the amphoteric rosin air-entraining agent of the present invention is as follows:

[0021]

[0022] Wherein, R is a straight chain alkane of 4 carbon atoms.

[0023] Example 1: The preparation method of the amphoteric rosin air-entraining agent of the present invention comprises the following process steps: ① 30g of rosin acid and 13.5g of modified substance A, namely N,N-dimethyl-1,3-propylenediamine, are added into a reactor, and 0.6g of NaF is used as a catalyst, 1g of aluminum oxide is used as a water absorbent, and the mixture is stirred and reacted at 155°C for 9h. After the obtained material is cooled, 150g of acetone is added, and the mixture is stirred, filtered and dried to obtain a solid intermediate product; ② 32g of the intermediate product, 20g of the modified substance B, and a solvent are added to a reactor, and the mixture is reacted at 75°C for 10h. The modified substance B is sodium chloroacetate, and the solvent is a combination of 119mL of methanol (about 94.2g) and 10g of water. After the reaction is completed, the solvent is distilled off under reduced pressure, 130g of ethyl acetate is added, and the mixture is stirred, filtered and dried to obtain the final product, which is an amphoteric rosin air-entraining agent; the mass ratio of the above-mentioned rosin acid to the modified substance A is 1:0.45, and the mass ratio of the rosin acid, sodium fluoride, aluminum oxide, and acetone is 1:0.02:0.033:5; the mass ratio of the above-mentioned intermediate product, the modified substance B, the solvent, and ethyl acetate is 1:0.625:3.26:4.06.

[0024] Example 2: The preparation method of the amphoteric rosin air-entraining agent of the present invention comprises the following process steps: ① 30g of rosin acid and 16g of modified substance A, namely N,N-dimethyl-1,3-propylenediamine, are added to a reactor, 1.8g of NaF is used as a catalyst, 2.6g of aluminum oxide is used as a water absorbent, and the reaction is stirred at 165°C for 10h. After the obtained material is cooled, 170g of acetone is added, and the solid intermediate product is obtained after stirring, filtering and drying; ② 38g of the intermediate product, 23g of modified substance B, and a solvent are added to a reactor, and the reaction is carried out at 79°C for 12h. The modified substance B is sodium chloroacetate, and the solvent is a combination of 150mL of ethanol (about 118.35g) and 30mL of water. After the reaction is completed, The solvent was distilled off under reduced pressure, 210 mL of ethyl acetate (about 189.42 g) was added, stirred, filtered and dried to obtain the final product, which was an amphoteric rosin air-entraining agent; the mass ratio of the above-mentioned rosin acid to the modifier A was 1:0.533, and the mass ratio of rosin acid, sodium fluoride, aluminum oxide and acetone was 1:0.06:0.087:5.67; the mass ratio of the above-mentioned intermediate product, modifier B, solvent and ethyl acetate was 1:0.61:3.9:4.98.

[0025] Example 3: The preparation method of the amphoteric rosin air-entraining agent of the present invention comprises the following process steps: ① 30g of rosin acid and 21g of modified substance A, namely N,N-dimethyl-1,3-ethylenediamine, are added into a reactor, and 2.8g of NaF is used as a catalyst, 0.9g of aluminum oxide is used as a water absorbent, and the mixture is stirred and reacted at 170°C for 15h. After the obtained material is cooled, 240mL of acetone (about 189.12g) is added, and the mixture is stirred, filtered and dried to obtain a solid intermediate product; ② 40g of the intermediate product, 27g of the modified substance B, and 240g of the solvent, i.e., isopropanol, are added to a reactor, and the mixture is reacted at 85°C for 15h. The modified substance B is sodium bromoacetate. After the reaction is completed, the solvent is distilled off under reduced pressure, 240g of ethyl acetate is added, and the mixture is stirred, filtered and dried to obtain the final product, i.e., an amphoteric rosin air-entraining agent; the mass ratio of the above-mentioned rosin acid to the modified substance A is 1:0.7, and the mass ratio of the rosin acid, sodium fluoride, aluminum oxide and acetone is 1:0.09:0.03:6.3; the mass ratio of the above-mentioned intermediate product, the modified substance B, the solvent and ethyl acetate is 1:0.675:6:6.

[0026] Example 4: The preparation method of the amphoteric rosin air-entraining agent of the present invention comprises the following process steps: ① 30g of rosin acid and 15g of modified substance A, namely N,N-dimethyl-1,3-butanediamine, are added to a reactor, and 0.9g of NaF is used as a catalyst and 3g of alumina is used as a water absorbent. The mixture is stirred and reacted at 150°C for 12h. After the obtained material is cooled, 190g of acetone is added. The mixture is stirred, filtered and dried to obtain a solid intermediate product. ② 35g of the intermediate product, 23g of the modified substance B and a solvent are added to a reactor and reacted at 75°C for 10h. The modified substance B is sodium chloroacetate, and the solvent is a combination of 90g of isopropanol and 150g of methanol. After the reaction is completed, the solvent is distilled off under reduced pressure, 180g of ethyl acetate is added, and the mixture is stirred, filtered and dried to obtain the final product, which is an amphoteric rosin air-entraining agent. The mass ratio of the above-mentioned rosin acid to the modified substance A is 1:0.5, and the mass ratio of the rosin acid, sodium fluoride, alumina and acetone is 1:0.03:0.1:6.33; the mass ratio of the above-mentioned intermediate product, the modified substance B, the solvent and ethyl acetate is 1:0.66:6.86:5.14.

[0027] Example 5: The preparation method of the amphoteric rosin air-entraining agent of the present invention comprises the following process steps: ① 30g of rosin acid and 21g of modified substance A, namely N,N-dimethyl-1,3-propylenediamine, are added into a reactor, and 2.6g of NaF is used as a catalyst, 2.5g of aluminum oxide is used as a water absorbent, and the mixture is stirred and reacted at 160°C for 8h. After the obtained material is cooled, 240g of acetone is added, and the mixture is stirred, filtered and dried to obtain a solid intermediate product; ② 60g of the intermediate product, 28g of the modified substance B, and a solvent are added to a reactor, and the mixture is reacted at 75°C for 8h. The modified substance B is sodium bromoacetate, and the solvent is a combination of 80g of isopropanol and 130g of ethanol. After the reaction is completed, the solvent is distilled off under reduced pressure, 190g of ethyl acetate is added, and the mixture is stirred, filtered and dried to obtain the final product, which is an amphoteric rosin air-entraining agent; the mass ratio of the above-mentioned rosin acid to the modified substance A is 1:0.7, and the mass ratio of the rosin acid, sodium fluoride, aluminum oxide, and acetone is 1:0.087:0.083:8; the mass ratio of the above-mentioned intermediate product, the modified substance B, the solvent, and ethyl acetate is 1:0.47:3.5:3.17.

[0028] The following is the test part of the present invention (performance test of the present invention):

[0029] Application Example 1: A commercially available rosin air-entraining agent product was selected: produced by Shijiazhuang Changan Yucai Building Materials Co., Ltd. The air-entraining agent used was the water-soluble high-efficiency concrete rosin air-entraining agent prepared in Example 1 of a water-soluble high-efficiency concrete rosin air-entraining agent and a preparation method thereof disclosed in CN106082764A.

[0030] Esheng P.O42.5 cement was used to prepare cement pore liquid. Cement and water were mixed at a water-cement ratio of 2:1, stirred for 2 minutes and then allowed to stand. The upper clear liquid was repeatedly filtered to obtain clear cement pore liquid. The comparative sample and the example product were dissolved in the cement pore liquid to prepare a solution with a mass fraction of 1%. The foaming performance and bubble stability of the air entraining agent solution were tested by the oscillation method.

[0031] Table 1 Solution state, foaming performance and foam stabilization performance of different air-entraining agent solutions

[0032]

[0033] It can be seen from Table 1 that, compared with the rosin air-entraining agent, the modified product does not produce flocculent precipitation after being dissolved in the cement pore liquid, and the initial foam height is higher. The ratio of the foam height at 5min and 10min to the initial foam height is larger, indicating that the amphoteric rosin air-entraining agent of the present invention has better salt resistance, foaming ability and foam stabilizing performance than the rosin air-entraining agent.

[0034] Application Example 2: The embodiment and the comparative sample were added into concrete for experiment. The concrete raw materials are as follows:

[0035] Cement: Esheng PO 42.5 cement; Sand: machine-made sand, fineness modulus 2.7; Stone: crushed pebbles with a particle size of 5-25 mm. Water: ordinary tap water. The admixture is a commercially available high-performance polycarboxylate water reducer. The commercially available high-performance polycarboxylate water reducer is a polyether polycarboxylate high-performance water reducer, and its synthesis process is as follows: ① Polymerization reaction: 220g of acrylic acid is measured, and 210g of deionized water is added, and pumped into titration tank A for standby (as A material). 2g of vitamin C, 7.60g of thioglycolic acid are measured, and 420g of deionized water are added, and pumped into titration tank B for standby (as B material). Add 2300g of deionized water and 1800g of allyl alcohol polyoxyethylene ether into the reactor, stir, raise the temperature from room temperature to 55°C, add 12.0g of hydrogen peroxide, titrate material A and material B at the same time, titrate material A in 2.5 hours, and material B in 3 hours, keep warm for 1.5 hours, control the temperature at 60±2°C, and obtain a polymer. ② Neutralization reaction: cool the polymer to below 50°C (45°C), add (30% by mass concentration) sodium hydroxide aqueous solution while stirring, adjust the pH value to 6-7, complete the reaction, and obtain a polyether polycarboxylic acid high-performance water reducer with a solid content of about 40%. The concrete formula is shown in Table 2.

[0036] Table 2 Concrete mix ratio

[0037]

[0038] The admixture dosage was adjusted so that the concrete slump was 180±5 mm, and the air entraining agent dosage was adjusted so that the air content of the concrete was controlled at 3.5%-4.0%. The test results are shown in Table 3.

[0039] Table 3 Test results

[0040]

[0041] It can be seen from Table 3 that, under the condition of controlling the initial air content to be approximately the same, the air-entraining agent produced by each embodiment of the present invention (referring to Embodiment 1 to Embodiment 5 in the above tables) has a lower dosage than the rosin air-entraining agent and a higher air content in 1h, which means that the air-entraining agent produced by each embodiment of the present invention has better air-entraining performance and gas stabilizing performance than the rosin air-entraining agent.

[0042] The term "amphiphilic" in the amphoteric rosin air-entraining agent of the present invention refers to surface activity and acid, alkali and salt resistance.

Claims

1. An amphoteric rosin air-entraining agent, characterized in that The structural formula of the amphoteric rosin air-entraining agent is as follows: Wherein, R is a straight chain alkane of 2 to 4 carbon atoms.

2. A method for preparing the amphoteric rosin air-entraining agent according to claim 1, characterized in that The method comprises the following process steps: ① adding rosin acid and modified substance A into a reactor, using NaF as a catalyst and aluminum oxide as a water absorbent, stirring and reacting at 150-170°C for 8-15h, adding acetone after cooling the obtained material, stirring, filtering and drying to obtain a solid intermediate product; ② adding the intermediate product, modified substance B and solvent into a reactor, reacting at 75-85°C for 8-15h, distilling off the solvent under reduced pressure after the reaction is completed, adding ethyl acetate, stirring, filtering and drying to obtain the final product, which is an amphoteric rosin air-entraining agent; The above-mentioned modified substance A is one of N,N-dimethyl-1,3-ethylenediamine, N,N-dimethyl-1,3-propylenediamine, and N,N-dimethyl-1,3-butylenediamine; the mass ratio of rosin acid to modified substance A is 1:0.4-0.7, and the mass ratio of rosin acid, sodium fluoride, aluminum oxide, and acetone is 1:(0.02-0.1):(0.02-0.1):(5-8); the above-mentioned modified substance B is one of sodium chloroacetate and sodium bromoacetate; the mass ratio of the intermediate product, modified substance B, solvent, and ethyl acetate is 1:(0.4-0.8):(3-7):(3-7).

3. The method for preparing the amphoteric rosin air-entraining agent according to claim 2, characterized in that The solvent in step ② is one or a combination of two raw materials selected from methanol, ethanol, isopropanol and water.

4. The method for preparing the amphoteric rosin air-entraining agent according to claim 2, characterized in that The method comprises the following process steps: ① adding 30g of rosin acid and 13.5g of a modified substance A, namely N,N-dimethyl-1,3-propylenediamine, into a reactor, taking 0.6g of NaF as a catalyst and 1g of aluminum oxide as a water absorbent, stirring and reacting at 155°C for 9h, adding 150g of acetone after the obtained material is cooled, stirring, filtering and drying to obtain a solid intermediate product; ② adding 32g of the intermediate product, 20g of a modified substance B and a solvent into a reactor, reacting at 75°C for 10h, wherein the modified substance B is sodium chloroacetate, and the solvent is a combination of two raw materials, namely 119mL of methanol and 10g of water, after the reaction is completed, the solvent is distilled off under reduced pressure, 130g of ethyl acetate is added, stirring, filtering and drying to obtain the final product, namely the amphoteric rosin air entraining agent.

5. The method for preparing the amphoteric rosin air-entraining agent according to claim 2, characterized in that The method comprises the following process steps: ① adding 30g of rosin acid and 16g of a modified substance A, namely N,N-dimethyl-1,3-propylenediamine, into a reactor, taking 1.8g of NaF as a catalyst and 2.6g of alumina as a water absorbent, stirring and reacting at 165°C for 10h, adding 170g of acetone after the obtained material is cooled, stirring, filtering and drying to obtain a solid intermediate product; ② adding 38g of the intermediate product, 23g of a modified substance B and a solvent into a reactor, reacting at 79°C for 12h, wherein the modified substance B is sodium chloroacetate, and the solvent is a combination of two raw materials, namely 150mL of ethanol and 30mL of water, and after the reaction is completed, the solvent is distilled off under reduced pressure, 210mL of ethyl acetate is added, stirring, filtering and drying to obtain the final product, namely the amphoteric rosin air entraining agent.

6. The method for preparing the amphoteric rosin air-entraining agent according to claim 2, characterized in that The method comprises the following process steps: ① adding 30g of rosin acid and 21g of a modified substance A, namely N,N-dimethyl-1,3-ethylenediamine, into a reactor, taking 2.8g of NaF as a catalyst and 0.9g of alumina as a water absorbent, stirring and reacting at 170°C for 15h, adding 240mL of acetone after the obtained material is cooled, stirring, filtering and drying to obtain a solid intermediate product; ② adding 40g of the intermediate product, 27g of a modified substance B and 240g of a solvent, namely isopropanol, into a reactor, reacting at 85°C for 15h, wherein the modified substance B is sodium bromoacetate, and after the reaction is completed, the solvent is distilled off by reduced pressure distillation, adding 240g of ethyl acetate, stirring, filtering and drying to obtain a final product, namely an amphoteric rosin air entraining agent.

7. The method for preparing the amphoteric rosin air-entraining agent according to claim 2, characterized in that The method comprises the following process steps: ① adding 30g of rosin acid and 15g of a modified substance A, namely N,N-dimethyl-1,3-butanediamine, into a reactor, taking 0.9g of NaF as a catalyst and 3g of alumina as a water absorbent, stirring and reacting at 150°C for 12h, adding 190g of acetone after the obtained material is cooled, stirring, filtering and drying to obtain a solid intermediate product; ② adding 35g of the intermediate product, 23g of a modified substance B and a solvent into a reactor, reacting at 75°C for 10h, wherein the modified substance B is sodium chloroacetate, and the solvent is a combination of two raw materials, namely 90g of isopropanol and 150g of methanol, after the reaction is completed, the solvent is distilled off under reduced pressure, 180g of ethyl acetate is added, stirring, filtering and drying to obtain the final product, namely the amphoteric rosin air entraining agent.

8. The method for preparing the amphoteric rosin air-entraining agent according to claim 2, characterized in that The method comprises the following process steps: ① adding 30g of rosin acid and 21g of a modified substance A, namely N,N-dimethyl-1,3-propylenediamine, into a reactor, taking 2.6g of NaF as a catalyst and 2.5g of alumina as a water absorbent, stirring and reacting at 160°C for 8h, adding 240g of acetone after the obtained material is cooled, stirring, filtering and drying to obtain a solid intermediate product; ② adding 60g of the intermediate product, 28g of a modified substance B and a solvent into a reactor, reacting at 75°C for 8h, wherein the modified substance B is sodium bromoacetate, and the solvent is a combination of two raw materials, namely 80g of isopropanol and 130g of ethanol, after the reaction is completed, the solvent is distilled off under reduced pressure, 190g of ethyl acetate is added, stirring, filtering and drying to obtain the final product, namely the amphoteric rosin air entraining agent.

Citation Information

Patent Citations

  • Water-soluble high-efficiency concrete rosin air entraining agent and preparation method thereof

    CN106082764A

  • Method for preparing novel composite concrete air entraining agent

    CN110104986A

  • Air entraining agent for concrete with fly ash and preparation method thereof

    CN101898880A

  • Rosinyl quaternary ammonium salt dimeric surfactant as well as preparation method and application thereof

    CN103599729A