Formaldehyde-free paper tube adhesive and preparation method thereof
Through the synergistic effect of the deld-free paper tube glue formula and vinyl acetate and maleic anhydride, the existing paper tube glue has been solved, and higher environmental protection and performance improvement has been achieved.
Patent Information
- Application Number
- CN202411474558.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-22
- Publication Date
- 2025-03-07
AI Technical Summary
Existing paper tube glue has shortcomings in water resistance and moisture resistance, and the use of formaldehyde is not conducive to environmental protection.
The formula of deld-free paper tube glue is adopted, including cold water, hot water, polyvinyl alcohol, pH adjuster, defoamer, corn starch and bactericide, and the water resistance and moisture resistance of paper tube glue is improved through the synergistic effect of vinyl acetate and maleic anhydride.
The water resistance and moisture resistance of paper tube glue is improved, avoiding the problem of moisture absorption and softening, and improving environmental protection.
Smart Images

Figure BDA0005095696660000061 
Figure BDA0005095696660000062
Abstract
Description
Technical Field
[0001] The invention relates to the field of materials, in particular to formaldehyde-free paper tube glue and a preparation method thereof. Background Art
[0002] Adhesive for paper tubes is commonly known as paper tube glue, paper tube glue, etc. It is a special adhesive for making various paper tubes, paper barrels, paper cans and related paper products. Paper, cloth, plastic film, metal foil and other thin and soft materials are often rolled into bundles to make paper tube core rolls. These paper tubes are generally made of kraft paper or other raw paper by mechanical rolling and bonding. The adhesive used is called paper tube glue.
[0003] With the rapid development of my country's economy, the demand for paper tubes in the fields of daily necessities, textiles, light industry, packaging, leather, etc. is increasing. Such as toilet paper core tubes, textile yarn tubes, cloth, paper products, leather, plastic film and other roll packaging paper tubes, etc.
[0004] Traditionally used paper tube (tube) adhesives mainly include gelatin, gelatinized starch (including oxidized starch and modified starch), polyvinyl alcohol formal liquid (107) adhesive, polyvinyl acetate emulsion (white latex), PVA solution, etc. Among them, gelatin and starch adhesives are basically not used due to low bonding strength and short storage period; the biggest disadvantage of polyvinyl alcohol adhesive is poor water resistance. The compressive strength of paper tubes decreases significantly with the increase of storage time. Although it can be partially improved after acetalization, the market is mainly through the addition of formaldehyde. In the process of preparing polyvinyl alcohol formal type paper tube adhesive, there are both intramolecular acetal and intermolecular acetal, which makes the colloid have a wider relative molecular mass distribution, which is conducive to improving bonding strength and accelerating drying speed.
[0005] However, the addition of formaldehyde is not conducive to environmental protection. The market needs a kind of adhesive that is both environmentally friendly and can improve the performance of paper tube glue, so that the paper tube glue has certain high temperature resistance, water resistance and moisture resistance, and avoids moisture absorption and softening. Summary of the invention
[0006] To address the deficiencies of the prior art, the present invention aims to provide a modified polyvinyl alcohol paper tube glue and a preparation method thereof. The formula and method of the present invention can simultaneously improve the performance of the paper tube glue, so that the paper tube glue has better water and moisture resistance.
[0007] In order to achieve the above object, the present invention adopts the following technical solution:
[0008] Formaldehyde-free paper tube glue includes: 3500-4000 parts of cold water, 1880 parts of kaolin, 25 parts of boric acid, 3000-4000 parts of hot water, 2488 500 parts of polyvinyl alcohol, 145-155 parts of pH regulator, 20 parts of defoamer, 50 parts of corn starch and 10 parts of bactericide.
[0009] The aforementioned formaldehyde-free paper tube glue includes: 3500-4000 parts of cold water, 1880 parts of kaolin, 25 parts of boric acid, 3000-4000 parts of hot water, 2488500 parts of polyvinyl alcohol, 145-155 parts of pH regulator, 20 parts of vinyl acetate, 10 parts of maleic anhydride, 20 parts of defoaming agent, 50 parts of corn starch, and 10 parts of bactericide.
[0010] The aforementioned formaldehyde-free paper tube glue, polyvinyl alcohol is: polyvinyl alcohol 2488.
[0011] The pH adjuster of the aforementioned formaldehyde-free paper tube glue is as follows: 133 parts of hydrochloric acid solution and 16 parts of ammonia water.
[0012] The aforementioned formaldehyde-free paper tube glue, the defoaming agent includes: one or a combination of silicone defoaming agent, mineral oil defoaming agent or polyether defoaming agent.
[0013] The aforementioned formaldehyde-free paper tube glue and bactericides include: hydrogen peroxide, alcohol, and hypochlorous acid water.
[0014] The preparation method of formaldehyde-free paper tube glue comprises the following steps:
[0015] Step 1, prepare acid: hydrochloric acid solution - weigh 950 kg of pure water in a ton barrel and slowly add 50 kg of original hydrochloric acid, stir evenly, label it, and set aside;
[0016] Step 2: Before starting the machine, check whether the equipment is normal, make sure there is no material in the kettle, and close the bottom valve.
[0017] Step 3, dissolution:
[0018] a. Add 3500Kg of cold water to the kettle and stir at 70°. After 5 minutes, add kaolin and stir for 2 hours.
[0019] b. Add 20 kg of glacial acetic acid, then slowly add 25 kg of boric acid; add 2488 polyvinyl alcohol after adding 3500 kg of hot water, and cover the manhole cover;
[0020] Step 4, heating: close the circulating water inlet valve and outlet valve of the 303A kettle, then fully open the steam trap and bypass valve, open the steam valve, fully open; after the steam water in the coil is drained, close the bypass valve; when the temperature reaches 70℃, adjust the stirring to 50, when the temperature rises to 87℃, close the steam valve and start timing, keep warm for 1 hour and 15 minutes;
[0021] Step 5, dilution: add 150 kg of cold water into a stainless steel barrel, start the high-speed disperser to stir, add 2 kg of defoamer, and stir thoroughly;
[0022] Step 6, adjust pH: first confirm that the feed pump and valve are opened correctly, then use a diaphragm pump to transfer a specified amount of hydrochloric acid solution into the R303A kettle, and adjust the pH to ≤3; after adjusting, flush the pipeline with 60 kg of flushing water;
[0023] Step 7. After adjusting the pH, make sure the valve is opened correctly before transfer and then start the pump for transfer. After the transfer is completed, rinse with 60KG of water and continue to heat up. When the temperature rises to 87°C, turn off the steam, start timing at 90°C, and react for 1 hour.
[0024] Step 8, adjust pH: slowly add appropriate amount of ammonia water and stir thoroughly; adjust the pH value in the kettle to between 4-4.2, and then prepare to cool down;
[0025] Step 9, gelatinization: After adjusting the pH, add the stirred starch solution, and start circulating cooling water to cool down 10 minutes after adding; flush the pipeline water with 30KG of reserved water;
[0026] Step 10, cooling: Close the steam trap, open the circulating water inlet valve and outlet valve, then start the circulating water pump to start cooling, making sure the front and rear inlet and outlet valves of the circulating water pump are open.
[0027] Step 11, post-treatment: when the temperature in the kettle drops below 45°C, add the remaining defoamer, bactericide and remaining reserved water.
[0028] Step 12, discharging: when the temperature in the kettle drops below 40°C, take samples for testing, and discharge the materials after the test is qualified.
[0029] The preparation method of the aforementioned formaldehyde-free paper tube glue comprises the following steps:
[0030] Step 1, prepare acid: hydrochloric acid solution - weigh 950 kg of pure water in a ton barrel and slowly add 50 kg of original hydrochloric acid, stir evenly, label it, and set aside;
[0031] Step 2: Before starting the machine, check whether the equipment is normal and make sure there is no material in the kettle; the bottom valve must be closed.
[0032] Step 3, dissolution:
[0033] a. Add 3500Kg of cold water to the kettle and stir at 70°. After 5 minutes, add kaolin and stir for 2 hours.
[0034] b. Add 20 kg of glacial acetic acid, then slowly add 25 kg of boric acid; add 2488 polyvinyl alcohol after adding 3500 kg of hot water, and cover the manhole cover;
[0035] Step 4, heating: close the circulating water inlet valve and outlet valve of the 303A kettle, then fully open the steam trap and bypass valve, open the steam valve, fully open; after the steam water in the coil is drained, close the bypass valve; when the temperature reaches 70℃, adjust the stirring to 50, when the temperature rises to 87℃, close the steam valve and start timing, keep warm for 1 hour and 15 minutes;
[0036] Step 5, diluting the cross-linking mixture: add 150 kg of cold water into a stainless steel barrel, start a high-speed disperser to stir, add 20 parts of vinyl acetate, 10 parts of maleic anhydride and 2 kg of defoamer, and stir thoroughly;
[0037] Step 6, adjust pH: first confirm that the feed pump and valve are opened correctly, then use a diaphragm pump to transfer a specified amount of hydrochloric acid solution into the R303A kettle, and adjust the pH to ≤3; after adjusting, flush the pipeline with 60 kg of flushing water;
[0038] Step 7, reaction: after pH adjustment, transfer the diluted cross-linking mixture in the stainless steel barrel to the 303A kettle. Before transfer, ensure that the valve is opened correctly and then start the pump for transfer. After the transfer is completed, rinse with 60KG of water and continue to heat up. When the temperature rises to 87°C, turn off the steam, start timing at 90°C, and react for 1 hour;
[0039] Step 8, adjust pH: slowly add appropriate amount of ammonia water and stir thoroughly; adjust the pH value in the kettle to between 4-4.2, and then prepare to cool down;
[0040] Step 9, gelatinization: After adjusting the pH, add the stirred starch solution, and start circulating cooling water to cool down 10 minutes after adding; flush the pipeline water with 30KG of reserved water;
[0041] Step 10, cooling: Close the steam trap, open the circulating water inlet valve and outlet valve, then start the circulating water pump to start cooling, making sure the front and rear inlet and outlet valves of the circulating water pump are open.
[0042] Step 11, post-treatment: when the temperature in the kettle drops below 45°C, add the remaining defoamer, bactericide and remaining reserved water.
[0043] Step 12, discharging: when the temperature in the kettle drops below 40°C, take samples for testing, and discharge the materials after the test is qualified.
[0044] The present invention is beneficial in that:
[0045] The present invention finds that vinyl acetate and maleic anhydride have a synergistic effect in improving the water and moisture resistance of paper tube glue. DETAILED DESCRIPTION
[0046] The present invention is described in detail below with reference to specific embodiments.
[0047] Embodiment 1:
[0048] Sample 1 was prepared according to the following preparation method and formula:
[0049] Step 1, prepare acid: hydrochloric acid solution - weigh 950 kg of pure water in a ton barrel and slowly add 50 kg of original hydrochloric acid, stir evenly, label it, and set aside;
[0050] Step 2: Before starting the machine, check whether the equipment is normal and make sure there is no material in the kettle; the bottom valve must be closed.
[0051] Step 3, dissolution:
[0052] a. Add 3500Kg of cold water to the kettle and stir at 70°. After 5 minutes, add kaolin and stir for 2 hours.
[0053] b. Add 20 kg of glacial acetic acid, then slowly add 25 kg of boric acid; add 2488 polyvinyl alcohol after adding 3500 kg of hot water, and cover the manhole cover;
[0054] Step 4, heating: close the circulating water inlet valve and outlet valve of the 303A kettle, then fully open the steam trap and bypass valve, open the steam valve, fully open; after the steam water in the coil is drained, close the bypass valve; when the temperature reaches 70℃, adjust the stirring to 50, when the temperature rises to 87℃, close the steam valve and start timing, keep warm for 1 hour and 15 minutes;
[0055] Step 5, diluting the cross-linking mixture: add 150 kg of cold water into a stainless steel barrel, start a high-speed disperser to stir, add 20 kg of vinyl acetate, 10 kg of maleic anhydride and 2 kg of defoamer, and stir thoroughly;
[0056] Step 6, adjust pH: first confirm that the feed pump and valve are opened correctly, then use a diaphragm pump to transfer a specified amount of hydrochloric acid solution into the R303A kettle, and adjust the pH to ≤3; after adjusting, flush the pipeline with 60 kg of flushing water;
[0057] Step 7. After pH adjustment, transfer the diluted cross-linking mixture in the stainless steel barrel to the 303A kettle. Before transfer, ensure that the valve is opened correctly and then start the pump for transfer. After the transfer is completed, rinse with 60KG of water and continue to heat up. When the temperature rises to 87°C, turn off the steam, start timing at 90°C, and react for 1 hour.
[0058] Step 8, adjust pH: slowly add appropriate amount of ammonia water and stir thoroughly; adjust the pH value in the kettle to between 4-4.2, and then prepare to cool down;
[0059] Step 9, gelatinization: After adjusting the pH, add the stirred starch solution, and start circulating cooling water to cool down 10 minutes after adding; flush the pipeline water with 30KG of reserved water;
[0060] Step 10, cooling: Close the steam trap, open the circulating water inlet valve and outlet valve, then start the circulating water pump to start cooling, making sure the front and rear inlet and outlet valves of the circulating water pump are open.
[0061] Step 11, post-treatment: when the temperature in the kettle drops below 45°C, add the remaining defoamer, bactericide and remaining reserved water.
[0062] Step 12, discharging: when the temperature in the kettle drops below 40°C, take samples for testing, and discharge the materials after the test is qualified.
[0063] Comparative Example 1 Obtain Comparative Sample 1:
[0064] The difference from Example 1 is that the cross-linked mixed liquid only contains vinyl acetate; Step 5, diluting the cross-linked mixed liquid: add 150 kg of cold water into a stainless steel barrel, start a high-speed disperser to stir, add 20 kg of vinyl acetate and 2 kg of defoaming agent, and stir thoroughly; the other steps are the same as in Example 1.
[0065] Comparative Example 2 Obtain Comparative Sample 2:
[0066] The difference from Example 1 is that the cross-linked mixed solution contains only maleic anhydride; Step 5, diluting the cross-linked mixed solution: add 150 kg of cold water into a stainless steel barrel, start a high-speed disperser to stir, add 10 kg of maleic anhydride and 2 kg of defoaming agent, and stir thoroughly; the other steps are the same as in Example 1.
[0067] Comparative Example 3 obtains comparative sample 3 acetal paper tube glue:
[0068] The difference from Example 1 is that maleic anhydride and vinyl acetate are not used, but formaldehyde is used.
[0069] Comparative Example 4:
[0070] Comparative sample 4 was prepared according to the following preparation method and formula:
[0071] The preparation method of formaldehyde-free paper tube glue comprises the following steps:
[0072] Step 1, prepare acid: hydrochloric acid solution - weigh 950 kg of pure water in a ton barrel and slowly add 50 kg of original hydrochloric acid, stir evenly, label it, and set aside;
[0073] Step 2: Before starting the machine, check whether the equipment is normal, make sure there is no material in the kettle, and close the bottom valve.
[0074] Step 3, dissolution:
[0075] a. Add 3500Kg of cold water to the kettle and stir at 70°. After 5 minutes, add kaolin and stir for 2 hours.
[0076] b. Add 20 kg of glacial acetic acid, then slowly add 25 kg of boric acid; add 2488 polyvinyl alcohol after adding 3500 kg of hot water, and cover the manhole cover;
[0077] Step 4, heating: close the circulating water inlet valve and outlet valve of the 303A kettle, then fully open the steam trap and bypass valve, open the steam valve, fully open; after the steam water in the coil is drained, close the bypass valve; when the temperature reaches 70℃, adjust the stirring to 50, when the temperature rises to 87℃, close the steam valve and start timing, keep warm for 1 hour and 15 minutes;
[0078] Step 5, dilution: add 150 kg of cold water into a stainless steel barrel, start the high-speed disperser to stir, add 2 kg of defoamer, and stir thoroughly;
[0079] Step 6, adjust pH: first confirm that the feed pump and valve are opened correctly, then use a diaphragm pump to transfer a specified amount of hydrochloric acid solution into the R303A kettle, and adjust the pH to ≤3; after adjusting, flush the pipeline with 60 kg of flushing water;
[0080] Step 7. After adjusting the pH, make sure the valve is opened correctly before transfer and then start the pump for transfer. After the transfer is completed, rinse with 60KG of water and continue to heat up. When the temperature rises to 87°C, turn off the steam, start timing at 90°C, and react for 1 hour.
[0081] Step 8, adjust pH: slowly add appropriate amount of ammonia water and stir thoroughly; adjust the pH value in the kettle to between 4-4.2, and then prepare to cool down;
[0082] Step 9, gelatinization: After adjusting the pH, add the stirred starch solution, and start circulating cooling water to cool down 10 minutes after adding; flush the pipeline water with 30KG of reserved water;
[0083] Step 10, cooling: Close the steam trap, open the circulating water inlet valve and outlet valve, then start the circulating water pump to start cooling, making sure the front and rear inlet and outlet valves of the circulating water pump are open.
[0084] Step 11, post-treatment: when the temperature in the kettle drops below 45°C, add the remaining defoamer, bactericide and remaining reserved water.
[0085] Step 12, discharging: when the temperature in the kettle drops below 40°C, take samples for testing, and discharge the materials after the test is qualified.
[0086] The difference between Comparative Example 4 and Example 1 is that maleic anhydride and vinyl acetate are not used.
[0087] Experiment 1: Test the performance of sample 1, formaldehyde-free paper tube glue and comparison sample 4, acetal paper tube glue:
[0088] The physical property comparison adopts the test of paper breaking effect, drying speed, wire drawing property, viscosity and other indicators. The viscosity test is based on GB / T2794-1995. The experimental results are shown in Table 1.
[0089] Table 1
[0090]
[0091] Experiment 2: Test water resistance. The samples were immersed in boiling water at 95-100℃, and the debonding phenomenon of the tube body was observed. The time for the tube body to completely debond was recorded. The test data is shown in Table 2.
[0092] Table 2
[0093]
[0094] It can be seen from this that the paper tube glue obtained by using vinyl acetate and maleic anhydride as cross-linking agents has a synergistic effect in water resistance.
[0095] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the above embodiments do not limit the present invention in any form, and any technical solution obtained by equivalent replacement or equivalent transformation falls within the protection scope of the present invention.
Claims
1. A formaldehyde-free paper tube glue, characterized in that: include: 3500-4000 parts of cold water, 1880 parts of kaolin, 25 parts of boric acid, 3000-4000 parts of hot water, 2488500 parts of polyvinyl alcohol, 145-155 parts of pH regulator, 20 parts of defoamer, 50 parts of corn starch, and 10 parts of bactericide.
2. The formaldehyde-free paper tube glue according to claim 1, characterized in that: include: 3500-4000 parts of cold water, 1880 parts of kaolin, 25 parts of boric acid, 3000-4000 parts of hot water, 2488500 parts of polyvinyl alcohol, 145-155 parts of pH regulator, 20 parts of vinyl acetate, 10 parts of maleic anhydride, 20 parts of defoamer, 50 parts of corn starch, and 10 parts of bactericide.
3. The formaldehyde-free paper tube glue according to claim 1, characterized in that: The polyvinyl alcohol is polyvinyl alcohol 2488.
4. The formaldehyde-free paper tube glue according to claim 1, characterized in that: The pH adjuster is: 133 parts of hydrochloric acid solution and 16 parts of ammonia water.
5. The formaldehyde-free paper tube glue according to claim 1, characterized in that: The defoamer includes: one or more of a polyether-modified silicone defoamer, a mineral oil defoamer or a polyether defoamer.
6. The formaldehyde-free paper tube adhesive according to claim 1, characterized in that: Fungicides include: Preventol IT3MV is a combination of one or more of hydrogen peroxide, alcohol or hypochlorous acid water.
7. A method for preparing formaldehyde-free paper tube glue, characterized in that: The steps include: Step 1, prepare acid: hydrochloric acid solution - weigh 950 kg of pure water in a ton barrel and slowly add 50 kg of original hydrochloric acid, stir evenly, label it, and set aside; Step 2: Before starting the machine, check whether the equipment is normal, make sure there is no material in the kettle, and close the bottom valve; Step 3, dissolution: a. Add 3500Kg of cold water to the kettle and stir until the mixing degree is 70%, the stirring speed is 110 rpm, and kaolin is added after 5 minutes and stirred for 2 hours; b. Add 20 kg of glacial acetic acid, then slowly add 25 kg of boric acid; add 2488 polyvinyl alcohol after adding 3500 kg of hot water, and cover the manhole cover; Step 4, heating: close the circulating water inlet valve and outlet valve of the 303A kettle, then fully open the steam trap and bypass valve, open the steam valve, fully open; after the steam water in the coil is drained, close the bypass valve; when the temperature reaches 70℃, adjust the stirring to 50, when the temperature rises to 87℃, close the steam valve and start timing, keep warm for 1 hour and 15 minutes; Step 5, dilution: add 150 kg of cold water into a stainless steel barrel, start the high-speed disperser to stir, add 2 kg of defoamer, and stir thoroughly; Step 6, adjust pH: first confirm that the feed pump and valve are opened correctly, then use a diaphragm pump to transfer a specified amount of hydrochloric acid solution into the R303A kettle, and adjust the pH to ≤3; after adjustment, flush the pipeline with 60 kg of flushing water; Step 7. After adjusting the pH, make sure the valve is opened correctly before transfer and then start the pump for transfer. After the transfer is completed, rinse with 60KG of water and continue to heat up. When the temperature rises to 87°C, turn off the steam, start timing at 90°C, and react for 1 hour. Step 8, adjust pH: slowly add appropriate amount of ammonia water and stir thoroughly; adjust the pH value in the kettle to between 4-4.2, and then prepare to cool down; Step 9, gelatinization: After adjusting the pH, add the stirred starch solution, and start circulating cooling water to cool down 10 minutes after adding; flush the pipeline water with 30KG of reserved water; Step 10, cooling: close the steam trap, open the circulating water inlet valve and outlet valve, and then start the circulating water pump to start cooling, making sure that the front and rear inlet and outlet valves of the circulating water pump are open; Step 11, post-treatment: when the temperature in the kettle drops below 45°C, add the remaining defoamer, bactericide and remaining reserved water; Step 12, discharging: when the temperature in the kettle drops below 40°C, take samples for testing, and discharge the materials after the test is qualified.
8. The method for preparing formaldehyde-free paper tube glue according to claim 7, characterized in that: The steps include: Step 1, prepare acid: hydrochloric acid solution - weigh 950 kg of pure water in a ton barrel and slowly add 50 kg of original hydrochloric acid, stir evenly, label it, and set aside; Step 2: Before starting the machine, check whether the equipment is normal and make sure there is no material in the kettle; the bottom valve must be closed; Step 3, dissolution: a. Add 3500Kg of cold water to the kettle and stir at 70°. After 5 minutes, add kaolin and stir for 2 hours. b. Add 20 kg of glacial acetic acid, then slowly add 25 kg of boric acid; add 2488 polyvinyl alcohol after adding 3500 kg of hot water, and cover the manhole cover; Step 4, heating: close the circulating water inlet valve and outlet valve of the 303A kettle, then fully open the steam trap and bypass valve, open the steam valve, fully open; after the steam water in the coil is drained, close the bypass valve; when the temperature reaches 70℃, adjust the stirring to 50, when the temperature rises to 87℃, close the steam valve and start timing, keep warm for 1 hour and 15 minutes; Step 5, diluting the cross-linking mixture: add 150 kg of cold water into a stainless steel barrel, start a high-speed disperser to stir and add 20 parts of vinyl acetate, 10 parts of maleic anhydride and 2 kg of defoamer, and stir thoroughly; Step 6, adjust pH: first confirm that the feed pump and valve are opened correctly, then use a diaphragm pump to transfer a specified amount of hydrochloric acid solution into the R303A kettle, and adjust the pH to ≤3; after adjusting, flush the pipeline with 60 kg of flushing water; Step 7, reaction: after pH adjustment, transfer the diluted cross-linking mixture in the stainless steel barrel to the 303A kettle. Before transfer, ensure that the valve is opened correctly and then start the pump for transfer. After the transfer is completed, rinse with 60KG of water and continue to heat up. When the temperature rises to 87°C, turn off the steam, start timing at 90°C, and react for 1 hour; Step 8, adjust pH: slowly add appropriate amount of ammonia water and stir thoroughly; adjust the pH value in the kettle to between 4-4.2, and then prepare to cool down; Step 9, gelatinization: After adjusting the pH, add the stirred starch solution, and start circulating cooling water to cool down 10 minutes after adding; flush the pipeline water with 30KG of reserved water; Step 10, cooling: close the steam trap, open the circulating water inlet valve and outlet valve, and then start the circulating water pump to start cooling, making sure that the front and rear inlet and outlet valves of the circulating water pump are open; Step 11, post-treatment: when the temperature in the kettle drops below 45°C, add the remaining defoamer, bactericide and remaining reserved water; Step 12, discharging: when the temperature in the kettle drops below 40°C, take samples for testing, and discharge the materials after the test is qualified.