CN101376639B - Method for coproduction of dispersants MF and sodium sulphite - Google Patents
Method for coproduction of dispersants MF and sodium sulphite Download PDFInfo
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- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 title claims abstract description 25
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 235000010265 sodium sulphite Nutrition 0.000 title abstract description 11
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 claims abstract description 48
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 32
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 32
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 17
- 238000009833 condensation Methods 0.000 claims abstract description 13
- 230000005494 condensation Effects 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000007864 aqueous solution Substances 0.000 abstract description 8
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract description 8
- 239000000243 solution Substances 0.000 abstract description 8
- 230000007935 neutral effect Effects 0.000 abstract description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 abstract description 4
- 235000011941 Tilia x europaea Nutrition 0.000 abstract description 4
- 239000004571 lime Substances 0.000 abstract description 4
- 239000002910 solid waste Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000008098 formaldehyde solution Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- WQHQCQSAAOGHQP-UHFFFAOYSA-N formaldehyde;2-methylnaphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=CC2=C(S(O)(=O)=O)C(C)=CC=C21 WQHQCQSAAOGHQP-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 239000000984 vat dye Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种生产分散剂MF并联产亚硫酸钠的方法,包括,在甲基萘原料中加入浓度95%以上的硫酸,通入三氧化硫进行磺化反应,三氧化硫充分反应后升温,抽真空,继续反应至溶液的总酸度22%~27%;磺化反应产生的二氧化硫气体用碱液吸收制备亚硫酸钠;磺化反应后的溶液加水调节缩合酸度至14%~20%后,加入甲醛水溶液进行缩合,缩合完毕后稀释,加碱调节pH值至中性,得到分散剂MF。本发明工艺不需要采用石灰来中和,因此不会产生硫酸钙等固体废弃物,质量能达到中国质量标准GB9294-88。同时,二氧化硫废气也得到了合理的回收利用,变废为宝,具有能耗低的特点,为清洁环保生产工艺。The invention discloses a method for producing dispersant MF and co-producing sodium sulfite, comprising: adding sulfuric acid with a concentration of more than 95% to the raw material of methylnaphthalene, feeding sulfur trioxide to carry out sulfonation reaction, and raising the temperature after the sulfur trioxide fully reacts , vacuumize, and continue to react until the total acidity of the solution is 22% to 27%; the sulfur dioxide gas produced by the sulfonation reaction is absorbed with lye to prepare sodium sulfite; the solution after the sulfonation reaction is added with water to adjust the condensation acidity to 14% to 20%, and then Formaldehyde aqueous solution is condensed, after the condensation is completed, it is diluted, and alkali is added to adjust the pH value to neutral to obtain the dispersant MF. The process of the invention does not need to use lime for neutralization, so solid wastes such as calcium sulfate will not be produced, and the quality can reach the Chinese quality standard GB9294-88. At the same time, sulfur dioxide waste gas has also been reasonably recycled, turning waste into treasure, featuring low energy consumption, and is a clean and environmentally friendly production process.
Description
技术领域technical field
本发明涉及一种磺化分散剂的制备方法,具体是指一种生产分散剂MF,同时联产亚硫酸钠的方法。The invention relates to a method for preparing a sulfonated dispersant, in particular to a method for producing the dispersant MF and simultaneously producing sodium sulfite.
背景技术Background technique
分散剂MF是国际上分散染料和还原染料最常用的一种染料分散剂,由于其具有很好的分散效果,且价格低廉而倍受亲睐。Dispersant MF is the most commonly used dye dispersant for disperse dyes and vat dyes in the world. It is popular because of its good dispersing effect and low price.
分散剂MF通常生产工艺是用工业甲基萘(甲基萘含量在60%以上)或者洗油(甲基萘含量在25%以上)经过与浓硫酸进行磺化、再与甲醛水溶液缩合、然后用石灰中和其残余的硫酸,通过氢氧化钠制碱,然后过滤掉硫酸钙等固体废弃物,得到甲基萘磺酸甲醛缩合物的水溶液,即分散剂MF。The usual production process of dispersant MF is to use industrial methylnaphthalene (methylnaphthalene content above 60%) or washing oil (methylnaphthalene content above 25%) to sulfonate with concentrated sulfuric acid, then condense with formaldehyde aqueous solution, and then Use lime to neutralize the residual sulfuric acid, make alkali through sodium hydroxide, and then filter off solid waste such as calcium sulfate to obtain an aqueous solution of methylnaphthalenesulfonic acid formaldehyde condensate, that is, dispersant MF.
现有工艺通常以98%的左右的浓硫酸作为磺化剂,其缺点是会产生大量的残余废酸,从而需要用石灰来中和,产生硫酸钙等固体废弃物,同时磺化会产生大量二氧化硫,从而影响环境。The existing technology usually uses about 98% concentrated sulfuric acid as the sulfonating agent, and its disadvantage is that it will produce a large amount of residual waste acid, which needs to be neutralized with lime, and solid waste such as calcium sulfate will be produced. At the same time, sulfonation will generate a large amount of sulfur dioxide, thereby affecting the environment.
公开号为CN1081451的中国发明专利通过用浓硫酸做磺化剂,用有机溶剂(通常为苯类取代物,如苯,甲苯等)共沸来磺化,然后利用缩合反应的循环物料调节其缩合酸度后进行缩合。该方法需要用循环物料调节酸度,且要回收有机溶剂,工艺较复杂,而且有机溶剂并非完全惰性,会消耗一定量的磺化剂,生成一定量的有害副产物,很难分离,从而影响产品质量。公开号为CN1043637的中国发明专利通过用二氧化硫做溶剂,用三氧化硫磺化,然后通过回收溶剂二氧化硫,用氮气除去残留的二氧化硫,该工艺要蒸发回收二氧化硫,同时二氧化硫需要冷却,需消耗大量能量,同时磺化产物中会有较多的残余二氧化硫,影响产物质量和环境,设备投资大,成本较高。The Chinese invention patent with the publication number CN1081451 uses concentrated sulfuric acid as a sulfonating agent, uses organic solvents (usually benzene substitutes, such as benzene, toluene, etc.) Acidity followed by condensation. This method needs to use recycled materials to adjust the acidity, and to recover the organic solvent, the process is more complicated, and the organic solvent is not completely inert, it will consume a certain amount of sulfonating agent, generate a certain amount of harmful by-products, which are difficult to separate, thus affecting the product quality. The Chinese invention patent with the publication number CN1043637 uses sulfur dioxide as a solvent, sulfonates it with sulfur trioxide, and then recovers the solvent sulfur dioxide and removes the residual sulfur dioxide with nitrogen. At the same time, there will be more residual sulfur dioxide in the sulfonated product, which will affect the product quality and the environment, and the equipment investment will be large and the cost will be high.
发明内容Contents of the invention
本发明提供了一种采用新的磺化工艺生产分散剂MF的方法,该方法工艺简单,不污染环境,在生产同时还可以联产亚硫酸钠,资源利用最大化。The invention provides a method for producing dispersant MF by adopting a new sulfonation process. The method has simple process, does not pollute the environment, and can also co-produce sodium sulfite during production, thereby maximizing resource utilization.
一种生产分散剂MF并联产亚硫酸钠的方法,包括,在甲基萘原料中加入浓度95%以上的硫酸,通入三氧化硫进行磺化反应,磺化反应温度为30~155℃,最优为50~100℃;三氧化硫充分反应后,135~155℃抽真空,继续反应至反应体系的总酸度22%~27%,23%~25%为最优;磺化反应产生的二氧化硫气体用碱液吸收制备亚硫酸钠;磺化反应后的溶液加水调节缩合酸度至14%~20%,最优为16%~18%,加入甲醛水溶液进行缩合,缩合反应的温度一般在80-120℃,压力一般不超过0.2Mpa;缩合完毕后加水稀释,加碱调节pH值至中性,得到甲基萘磺酸甲醛缩合物的水溶液,即分散剂MF。A method for producing dispersant MF and co-producing sodium sulfite, comprising: adding sulfuric acid with a concentration of more than 95% to the methylnaphthalene raw material; The optimum temperature is 50-100°C; after the sulfur trioxide is fully reacted, vacuumize at 135-155°C, and continue to react until the total acidity of the reaction system is 22%-27%, and 23%-25% is the optimum; the sulfur dioxide produced by the sulfonation reaction The gas is absorbed with lye to prepare sodium sulfite; add water to the solution after sulfonation reaction to adjust the condensation acidity to 14%-20%, the optimal value is 16%-18%, and add formaldehyde aqueous solution for condensation. The temperature of condensation reaction is generally 80-120°C , the pressure generally does not exceed 0.2Mpa; after the condensation is completed, add water to dilute, add alkali to adjust the pH value to neutral, and obtain an aqueous solution of methyl naphthalenesulfonic acid formaldehyde condensate, that is, the dispersant MF.
生产分散剂MF的主要反应式如下:The main reaction formula for producing dispersant MF is as follows:
(1)磺化(1) Sulfonation
(2)缩合:(2) Condensation:
(3)中和:(3) Neutralization:
所述的甲基萘原料可采用纯的甲基萘,但为降低生产成本,最优采用工业甲基萘或者洗油。所述的工业甲基萘的甲基萘含量在60%以上,所述得洗油的甲基萘含量在25%以上。当采用工业甲基萘时,反应中各物质的重量比工业甲基萘:硫酸:三氧化硫:甲醛=1:0.3~0.45:0.3~0.45:0.12~0.24,优选工业甲基萘:硫酸:三氧化硫:甲醛=1:0.35~0.40:0.35~0.40:0.15~0.20;当采用洗油时,反应中各物质的重量比洗油:硫酸:三氧化硫:甲醛=0.9:0.3~0.45:0.3~0.45:0.12~0.24,优选洗油:硫酸:三氧化硫:甲醛=0.9:0.35~0.40:0.35~0.40:0.15~0.20。The raw material of methylnaphthalene can be pure methylnaphthalene, but in order to reduce the production cost, industrial methylnaphthalene or wash oil is optimally used. The methylnaphthalene content of the industrial methylnaphthalene is more than 60%, and the methylnaphthalene content of the washing oil is more than 25%. When adopting industrial methyl naphthalene, the weight ratio industrial methyl naphthalene of each substance in the reaction: sulfuric acid: sulfur trioxide: formaldehyde=1: 0.3~0.45:0.3~0.45:0.12~0.24, preferred industrial methyl naphthalene: sulfuric acid: Sulfur trioxide: formaldehyde=1:0.35~0.40:0.35~0.40:0.15~0.20; when adopting wash oil, the weight ratio of each substance in the reaction wash oil: sulfuric acid: sulfur trioxide: formaldehyde=0.9:0.3~0.45: 0.3~0.45:0.12~0.24, preferably washing oil: sulfuric acid: sulfur trioxide: formaldehyde=0.9:0.35~0.40:0.35~0.40:0.15~0.20.
在本发明方法的反应过程中,甲基萘和浓硫酸、三氧化硫第一次磺化反应充分后,升高磺化温度,同时通过抽真空脱水,可以使浓硫酸较为充分的反应,反应完毕后,溶液中仅存极少量的硫酸。In the reaction process of the inventive method, after the first sulfonation reaction of methylnaphthalene, concentrated sulfuric acid and sulfur trioxide is sufficient, the sulfonation temperature is increased, and simultaneously by vacuum dehydration, the concentrated sulfuric acid can be relatively fully reacted, and the reaction After finishing, there is only a very small amount of sulfuric acid in the solution.
磺化产生的二氧化硫气体通过碱液吸收至pH值4~9,最优为5~7,然后再加碱调节pH值至11~13,此时再过滤除杂,蒸发浓缩,干燥得到的亚硫酸钠含量可在96%以上。Sulfur dioxide gas produced by sulfonation is absorbed by alkali solution to pH 4-9, the optimal value is 5-7, then add alkali to adjust pH value to 11-13, then filter to remove impurities, evaporate and concentrate, and dry the obtained sodium sulfite The content can be above 96%.
所述的碱液和碱最优使用氢氧化钠,虽然也可使用碳酸钠、碳酸氢钠等,但是反应过程中会产生温室气体二氧化碳。Described lye and alkali optimally use sodium hydroxide, although sodium carbonate, sodium bicarbonate etc. can also be used, but can produce greenhouse gas carbon dioxide in the reaction process.
和常规工艺相比,本发明工艺不需要采用石灰来中和,因此不会产生硫酸钙等固体废弃物,同时具有钙镁离子含量低的优点,由于残余游离硫酸较少,所以硫酸钠的含量一般在5%以下,质量能达到中国质量标准GB9294-88。同时,二氧化硫废气也得到了合理的回收利用,变废为宝,具有能耗低的特点,为清洁环保生产工艺。Compared with the conventional process, the process of the present invention does not need to use lime to neutralize, so solid wastes such as calcium sulfate will not be produced, and it has the advantage of low calcium and magnesium ion content. Since the residual free sulfuric acid is less, the content of sodium sulfate Generally below 5%, the quality can reach the Chinese quality standard GB9294-88. At the same time, sulfur dioxide waste gas has also been reasonably recycled, turning waste into treasure, featuring low energy consumption, and is a clean and environmentally friendly production process.
具体实施方式Detailed ways
实施例1Example 1
将60g工业甲基萘投入反应容器中,加入98%的浓硫酸23g,搅拌均匀,然后缓慢通入三氧化硫气体约25g,控制反应温度在50~60℃,通入时间控制在1~2小时,通毕,保温反应1小时后,升温至150℃,抽真空,控制真空度在0.025Mpa左右,在该温度下反应3小时,然后取样测量酸值,酸度合格后,降温到110℃,加入一定量的水,调节缩合酸度至18%,然后降温到70℃加入27g甲醛水溶液(一般浓度为36%~38%),升温到110℃加压反应5小时,然后降温降压,加水稀释,加氢氧化钠调pH值至中性,即得分散剂MF的水溶液,烘干得固体粉末MF。Put 60g of industrial methylnaphthalene into the reaction vessel, add 23g of 98% concentrated sulfuric acid, stir evenly, then slowly pass in about 25g of sulfur trioxide gas, control the reaction temperature at 50-60°C, and control the passage time at 1-2 Hours, pass through, heat preservation reaction for 1 hour, heat up to 150°C, vacuumize, control the vacuum degree at about 0.025Mpa, react at this temperature for 3 hours, then take samples to measure the acid value, after the acidity is qualified, cool down to 110°C, Add a certain amount of water to adjust the condensation acidity to 18%, then lower the temperature to 70°C and add 27g of formaldehyde solution (general concentration is 36% to 38%), heat up to 110°C and pressurize for 5 hours, then lower the temperature and pressure, add water to dilute , add sodium hydroxide to adjust the pH value to neutral, and obtain the aqueous solution of dispersant MF, and dry it to obtain solid powder MF.
磺化产生的二氧化硫气体用15%氢氧化钠溶液吸收至pH值为5.5,加入氢氧化钠使吸收后的碱液pH值为13,过滤除杂,蒸发浓缩,干燥后得到含量为96%以上的商品亚硫酸钠。The sulfur dioxide gas produced by sulfonation is absorbed with 15% sodium hydroxide solution until the pH value is 5.5, and sodium hydroxide is added to make the pH value of the absorbed lye 13, filtered to remove impurities, concentrated by evaporation, and dried to obtain a content of more than 96%. commercial sodium sulfite.
实施例2Example 2
将60g洗油投入反应容器中,加入98%的浓硫酸24g,搅拌均匀,然后缓慢通入三氧化硫气体约26g,控制反应温度在70~80℃,通入时间控制在2~3小时,通毕,保温反应1小时,开始升温至140℃,抽真空,控制真空度在0.02Mpa左右,在该温度下反应3小时,然后取样测量酸值,酸度合格后,降温到100℃,加入一定量的水,调节缩合酸度至20%,然后降温到70℃加入26g甲醛水溶液(一般浓度为36%~38%),升温到110℃加压反应5小时,然后降温降压,加水稀释,加氢氧化钠调pH值至中性,即得分散剂MF的水溶液,烘干得固体粉末MF。Put 60g of washing oil into the reaction vessel, add 24g of 98% concentrated sulfuric acid, stir evenly, then slowly feed about 26g of sulfur trioxide gas, control the reaction temperature at 70-80°C, and control the feeding time at 2-3 hours, After passing through, keep warm for 1 hour, start to heat up to 140°C, vacuumize, control the vacuum degree at about 0.02Mpa, react at this temperature for 3 hours, then take samples to measure the acid value, after the acidity is qualified, cool down to 100°C, add certain Amount of water, adjust the condensation acidity to 20%, then lower the temperature to 70°C, add 26g of formaldehyde solution (general concentration is 36%~38%), raise the temperature to 110°C and pressurize for 5 hours, then lower the temperature and reduce the pressure, add water to dilute, add Adjust the pH value to neutral with sodium hydroxide to obtain the aqueous solution of dispersant MF, and dry it to obtain solid powder MF.
磺化产生的二氧化硫气体用15%氢氧化钠溶液吸收至pH值为7,加入氢氧化钠使吸收后的碱液pH值为11,过滤除杂,蒸发浓缩,干燥后得到含量为96%以上的商品亚硫酸钠。The sulfur dioxide gas produced by sulfonation is absorbed with 15% sodium hydroxide solution until the pH value is 7, and sodium hydroxide is added to make the pH value of the absorbed lye solution 11, filtered to remove impurities, concentrated by evaporation, and dried to obtain a content of more than 96%. commercial sodium sulfite.
实施例3Example 3
将60g工业甲基萘投入反应容器中,加入98%的浓硫酸24g,搅拌均匀,然后缓慢通入三氧化硫气体约24g,控制反应温度在80~90℃,通入时间控制在2~3小时,通毕,保温反应1小时,开始升温至145℃,抽真空,控制真空度在0.03Mpa左右,在该温度下反应3小时,然后取样测量酸值,酸度合格后,降温到110℃,加入一定量的水,调节缩合酸度至15%,然后降温到70℃加入28g甲醛水溶液(一般浓度为36%~38%),升温到110℃加压反应5小时,然后降温降压,加水稀释,加氢氧化钠调pH值至中性,即得分散剂MF的水溶液,烘干得固体粉末MF。Put 60g of industrial methylnaphthalene into the reaction vessel, add 24g of 98% concentrated sulfuric acid, stir evenly, then slowly pass in about 24g of sulfur trioxide gas, control the reaction temperature at 80-90°C, and control the passage time at 2-3 Hours, pass through, heat preservation reaction for 1 hour, start to heat up to 145°C, vacuumize, control the vacuum degree at about 0.03Mpa, react at this temperature for 3 hours, then take samples to measure the acid value, after the acidity is qualified, cool down to 110°C, Add a certain amount of water to adjust the condensation acidity to 15%, then lower the temperature to 70°C and add 28g of formaldehyde solution (general concentration is 36% to 38%), heat up to 110°C and pressurize for 5 hours, then lower the temperature and pressure, add water to dilute , add sodium hydroxide to adjust the pH value to neutral, and obtain the aqueous solution of dispersant MF, and dry it to obtain solid powder MF.
磺化产生的二氧化硫气体用15%氢氧化钠溶液吸收至pH值为7.5,加入氢氧化钠使吸收后的碱液pH值为12,过滤除杂,蒸发浓缩,干燥后得到含量为96%以上的商品亚硫酸钠。The sulfur dioxide gas produced by sulfonation is absorbed with 15% sodium hydroxide solution until the pH value is 7.5, and sodium hydroxide is added to make the pH value of the absorbed lye 12, filtered to remove impurities, concentrated by evaporation, and dried to obtain a content of more than 96%. commercial sodium sulfite.
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CN101543746B (en) * | 2009-05-06 | 2012-06-27 | 北京华中新工贸有限公司 | Dispersant and preparation method thereof |
CN102114396A (en) * | 2010-12-10 | 2011-07-06 | 江阴市盛通化工有限公司 | Non-quinoline dispersant MF and production process |
RU2502671C1 (en) * | 2012-07-13 | 2013-12-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Башкирский государственный университет" | Method of obtaining sodium sulfate |
CN102746196B (en) * | 2012-07-17 | 2013-11-20 | 浙江闰土股份有限公司 | Sulfonating technique for producing dye dispersant MF (melamine-formaldehyde) |
CN103360285A (en) * | 2013-07-09 | 2013-10-23 | 安阳市双环助剂有限责任公司 | Production technology of dispersing agent MF (melamine-formaldehyde resin) |
CN104860851A (en) * | 2015-05-20 | 2015-08-26 | 上虞市力德助剂有限公司 | Preparation method of saline and alkali tolerant dispersing agent |
CN106397281A (en) * | 2015-07-28 | 2017-02-15 | 江苏吉华化工有限公司 | Dye dispersing agent production method |
CN105294514A (en) * | 2015-09-16 | 2016-02-03 | 浙江奇彩环境科技有限公司 | Improved production technology for preparing diffusant |
CN105541672B (en) * | 2015-12-15 | 2017-06-20 | 浙江闰土研究院有限公司 | A kind of process for cleanly preparing of dye dispersant MF |
CN106673017A (en) * | 2017-02-17 | 2017-05-17 | 四川省中明环境治理有限公司 | Environment-friendly production method for preparing sodium sulfite by utilizing sulfur to reduce waste sulfuric acid |
CN111689879A (en) * | 2020-06-03 | 2020-09-22 | 浙江五龙新材股份有限公司 | Clean production method of dispersing agent |
CN112375019A (en) * | 2020-11-25 | 2021-02-19 | 济宁碳素集团有限公司 | Method for producing environment-friendly low-quinoline MF dispersant by using ethylene tar |
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