- NEW METHOD FOR PRODUCING 2-ACRYLAMIDO-2-METHYLPROPANE SULPHONIC ACID
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The present invention relates to a production process for 2-acrylamido-2-methylpropane sulfonic acid including at least the following successive steps: 1) mixing of acrylonitrile with at least one compound contributing SO3 at a temperature included between ?80 and 30° C.;2) placing in contact and mixing isobutylene and the sulfonating mixture with a molar ratio of SO3 to isobutylene included between 0.2:1 and 2:1 and a molar ratio of acrylonitrile to isobutylene included between 3:1 and 60:1 at a temperature included between ?40 and 100° C.;3) solid/liquid separation of the reaction mixture and isolation of the solid particles in the form of a composition 1;4) mixing composition 1 at the end of step 3) with an aqueous solution A included at a temperature comprised between ?20 and 70° C. in order to obtain a suspension 1 of 2-acrylamido-2-methylpropane sulfonic acid crystals;5) solid/liquid separation of the suspension 1 and isolation of the crystals in form of composition 2.
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Paragraph 0123-0144
(2020/02/10)
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- HYDRATED CRYSTALLINE FORM OF 2-ACRYLAMIDO-2-METHYLPROPANE SULFONIC ACID
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The present invention relates to a hydrated crystalline form of 2-acrylamido-2-methylpropane sulfonic acid having a 2-theta powder X-ray diffraction diagram comprising peaks at 10.58°, 11.2°, 12.65°, 13.66°, 16.28°, 18.45°, 20°, 20.4°, 22.5°, 25.5°, 25.88°, 26.47°, 28.52°, 30.28°, 30.8°, 34.09°, 38.19°, 40.69°, 41.82°, 43.74°, 46.04° degrees (+/?0.1°). The present invention also relates to a production method for this form of 2-acrylamido-2-methylpropane sulfonic acid and a preparation method for an aqueous solution A of a salt of this form of 2-acrylamido-2-methylpropane sulfonic acid, and the (co)polymer of this form of -acrylamido-2-methylpropane sulfonic acid.
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Paragraph 0194-0196
(2020/02/15)
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- A 2 - acrylamide - 2 - methyl (alkanes) sulfonic acid
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The invention relates to a preparation method of 2-acrylamido-2-methylpropane sulfonic acid, and belongs to the field of organic synthesis and preparation. The preparation method comprises the steps of (1) adding acrylonitrile in a liquid-preparing kettle, cooling, and adding fuming sulfuric acid to obtain a mixed solution of acrylonitrile and sulfuric acid; (2) transferring partial mixed solution into a feed tank with a constant temperature for use, adding the residual mixed solution into a reaction kettle, adding an organic acid, heating, introducing isobutene, adding the standby mixed solution of acrylonitrile and sulfuric acid and controlling a temperature, a feed time and speed; (3) when isobutene is completely introduced, stirring while keeping the temperature, cooling, centrifuging or filtering to separate coarse crystals of a generated product and pumping a filtrate into a storage tank; (4) mixing the coarse crystals of the product with acrylonitrile under stirring, separating by centrifugation, drying in vacuum to obtain a product of 2-acrylamido-2-methylpropane sulfonic acid and pumping the filtrate into the storage tank; and (5) merging the filtrates, contacting the mixed filtrate with quicklime, and distilling to recycle acrylonitrile. The product provided by the invention has high purity and high polymerization activity and is liable to obtain a polymer with relatively high molecular weight.
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Paragraph 0025; 0026; 0027; 0028; 0029-0045; 0052
(2018/04/03)
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- METHOD FOR PRODUCING THE 2-ACRYLAMIDO-2-METHYLPROPANE SULFONIC ACID MONOMER AND POLYMER COMPRISING SAID MONOMER
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The invention relates to a method for producing 2-acrylamido-2-methylpropane sulfonic acid. Said method consists in reacting together acrylonitrile, fuming sulfuric acid and isobutylene. It is characterized in that the isobutylene contains less than 1000 ppm of butadiene and less than 1000 ppm of butene.
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Paragraph 0057; 0060; 0058; 0059; 0060
(2018/09/16)
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- Process for reducing sulfate ions in synthesis process of 2-acrylamido-2-methylpropanesulfonic acid
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The invention discloses a process for reducing sulfate ions in the synthesis process of 2-acrylamido-2-methylpropanesulfonic acid. The process comprises the following steps: (1) firstly, adding certain parts of acrylonitrile and a dehydrant into a reaction kettle, and supplying cooling water to cool to minus 30 DEG C to 0 DEG C; (2) introducing gasified isobutene into the reaction kettle at minus 30 DEG C to 0 DEG C, introducing a certain amount of the component, and continuously introducing isobutene and dropping fuming sulfuric acid at the same time; (3) after the fuming sulfuric acid is completely added, continuously introducing a certain amount of an isobutene gas; (4) after the material is completely added, performing heat-preservation reaction at 10-40 DEG C; and (5) performing cooling crystallization on a generated paste product, and performing separation drying, thereby obtaining a 2-acrylamido-2-methylpropanesulfonic acid synthesized product. The synthesized product disclosed by the invention is high in purity, low in cost, convenient in industrial production and relatively low in sulfate radical residue without refining.
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Paragraph 0033-0060
(2017/09/13)
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- A 2-acrylamide-2-methylpropane-sulfonic acid process for the continuous production of
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The invention provides a method for continuous production of 2-acryloylamino-2-methyl propanesulfonic acid. The method comprises the steps: acrylonitrile and sulfur trioxide are continuously mixed, the mixed liquid flows into a first-level reactor and is subjected to a first-level reaction with isobutene simultaneously introduced into the first-level reactor, the reaction liquid of the first-level reactor enters a second-level reactor and is subjected to a second-level reaction with isobutene and sulfur trioxide simultaneously introduced into the second-level reactor, then the reaction liquid of the second-level reactor is subjected to solid-liquid separation, and the obtained solid is dried to obtain the 2-acryloylamino-2-methyl propanesulfonic acid product. The occurrence of side reactions can be effectively reduced by adopting sulfur trioxide as a sulphonating agent, and the molecular weight of a polymer obtained from polymerization of the obtained 2-acryloylamino-2-methyl propanesulfonic acid as a monomer is relatively high. In addition, the continuous synthesis mode can effectively reduce possibly produced adverse effects on the stability of the product quality in the operation process, so as to further improve the product yield and quality.
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Paragraph 0026-0028
(2017/03/17)
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- Preparation method for 2-acrylamido-2-methylpropanesulfonic acid
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The invention provides a preparation method for 2-acrylamido-2-methylpropanesulfonic acid. The preparation method comprises a step of subjecting acrylonitrile, isobutene and oleum to a reaction under the action of sulfur-containing organic acid so as to obtain 2-acrylamido-2-methylpropanesulfonic acid. According to the method, sulfur-containing organic acid is used in the process of the reaction and can form mixed anhydride with oleum; HOS separated from the mixed anhydride has electrophilic activity and reacts with isobutene to form carbocation with a sulfo group; and the carbocation with the sulfo group reacts with acrylonitrile under the action of sulfuric acid so as to form 2-acrylamido-2-methylpropanesulfonic acid. 2-acrylamido-2-methylpropanesulfonic acid prepared by using the method has good purity and chroma. Experimental results show that a finished 2-acrylamido-2-methylpropanesulfonic acid product prepared by using the method has a purity of more than 99% and chroma of 15 to 18.
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Paragraph 0045; 0046
(2017/02/17)
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- A 2-acrylamide-2-methyl propanesulfonic acid production method
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The invention discloses a method for producing a 2-acrylamido-2-methylpropanesulfonic acid. The method comprises the steps: mixing acetic acid with water, then mixing with a crude 2-acrylamido-2-methylpropanesulfonic acid with the mass content of 90-95%, keeping the temperature constant during the mixing process, and thus obtaining a dissolved solution; and then continuously introducing the prepared dissolved solution into a crystallizer, discharging crystals from an outlet of the crystallizer to obtain the 2-acrylamido-2-methylpropanesulfonic acid with the mass content of 98% or more. An oil field temperature-resistant and salt-resistant polymer formed by polymerization of the 2-acrylamido-2-methylpropanesulfonic acid produced by the method and acrylamide can achieve relatively high molecular weight and can be better applied in the oil field exploration field.
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Paragraph 0034; 0035; 0036
(2017/01/02)
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- A 2-acrylamide-2-methyl propanesulfonic acid method for refining the crude product and its product
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The invention discloses a refining method of a 2-acrylamidyl-2-methul propanesulfonic acid coarse product and a product thereof. The method comprises the following steps: (1) mixing and contacting the 2-acrylamidyl-2-methul propanesulfonic acid coarse product with glacial acetic acid and heating to 80-105 DEG C to obtain a solid-liquid mixture, wherein the mass ratio of the 2-acrylamidyl-2-methul propanesulfonic acid coarse product and the glacial acetic acid is 1:(2-7); (2) mixing the obtained solid-liquid mixture obtained in the step (1) with deionized water, wherein solid in the solid-liquid mixture is fully dissolved within 3-12 minutes, and the use level of deionized water is 1-2 times of that required to fully dissolving the 2-acrylamidyl-2-methul propanesulfonic acid coarse product; and (3) cooling the liquor obtained in the step (2), cooling and crystallizing and carrying out solid-liquid separation. The method disclosed by the invention greatly improves the molecular weight of a polymer polymerized by the refined 2-acrylamidyl-2-methul propanesulfonic acid coarse product, and the demand on high temperature resistance and salt resistance of the polymer in tertiary oil recovery can be satisfied.
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Paragraph 0032; 0033; 0034; 0035; 0036; 0037
(2017/03/08)
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- 2-acrylamide-2-methyl propanesulfonic acid preparation method
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The invention discloses a preparation method of 2-acrylamido-2-methyl propane sulfonic acid, which comprises the following steps: placing 405 parts of acrylonitrile in a sealed reaction vessel I, adding 78.2 parts of oleum in the sealed reaction vessel I drop by drop, controlling the temperature at -5-0 DEG C to obtain a mixed liquid, adding drop by drop in a sealed reaction vessel II with rate of 1-5 parts/min, heating after dropping for 20-25 minutes and introducing 44.9 parts of isobutene with rate of 0.1-0.6 parts/min, controlling the temperature at 38-40 DEG C until addition of isobutene and the mixed liquor is completed, insulating for 1 hour, cooling to the temperature of 15 DEG C, performing pumping filtration after cooling for 1 hour, drying under vacuum for 2 hours at the temperature of 70-90 DEG C to obtain the methyl propane sulfonic acid (AMPS) crude product, adding acetic acid for refining, wherein the mass ratio of AMPS crude product to acetic acid is 1:3.7-4, performing reduced pressure distillation, performing pumping filtration, and drying to obtain the AMPS finished product. According to the invention, oleum is mixed with acrylonitrile in advance at the temperature of -5-0 DEG C, the color of the product is light. The preparation method is characterized in that the mixed liquid of oleum and acrylonitrile is introduced in the reaction vessel II with isobutene simultaneously, the generation of sulfonated acrylonitrile is inhibited, and the purity of product is increased.
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Paragraph 0037; 0042; 0043
(2017/04/08)
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- PURIFICATION METHOD OF N-tert-BUTYLACRYLAMIDE
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PROBLEM TO BE SOLVED: To provide a purification method performed under specific conditions which, when purifying N-tert-butylacrylamide (TBAM) by a sublimation method, can provide TBAM of high purity with little impurity contained in TBAM after purification and little coloration. SOLUTION: The purification method of TBAM comprises: separating from a reaction mixture 2-acrylamido-2-propanesulfonic acid obtained by reacting acrylonitrile, sulfuric acid, and isobutylene; recovering byproduct TBAM contained in the reaction mixture after the separation as crude crystals; and thereafter subliming the crude crystals from a molten liquid of 135 to 160°C under 600 Torr or less, and cooling the sublimation gas in stages in the order of 130 to 150°C at the outlet of a melting tank, 80 to 100°C at an upper part of a sublimation and collection tower, and 40 to 60°C at a lower part of the sublimation and collection tower. A content of the impurity, 3,3'-iminopropionitrile, in TBAM is 1000 ppm or less. COPYRIGHT: (C)2015,JPOandINPIT
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Paragraph 0038
(2020/10/10)
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- Identification of small molecule sulfonic acids as ecto-5'-nucleotidase inhibitors
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Ecto-5'-Nucleotidase inhibitors have great potential as anti-tumor agents. We have investigated biochemical properties of human and rat ecto-5'-Nucleotidases and characterized 19 small molecule sulfonic acid derivatives as potential inhibitors of ecto-5'-Nucleotidases. We identified 11 potent inhibitors of human and rat ecto-5'-Nucleotidases and checked their selectivity. Compound 10 (Sodium 2,4-dinitrobenzenesulfonate) with Ki value of 0.66 μM and 19 (N-(4- sulfamoylphenylcarbamothioyl) pivalamide) with Ki value of 0.78 μM were identified as the most potent inhibitors for human and rat ecto-5'-Nucleotidase, respectively. The present compounds have low molecular weights, water solubility and equal potency as compared to the reported inhibitors.
- Raza, Rabia,Saeed, Aamer,Lecka, Joanna,Sévigny, Jean,Iqbal, Jamshed
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p. 1133 - 1139
(2013/01/15)
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- 2-ACRYLAMIDE-2-METHYLPROPANESULFONIC ACID AND PROCESS FOR PRODUCING THE SAME
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A process for producing 2-acrylamide-2-methyl propane sulfonic acid (ATBS) which comprises reacting acrylonitrile, fuming sulfuric acid, and isobutylene. During the reaction, the concentration of 2-methyl-2-propenyl-1-sulfonic acid (IBSA) and/or that of 2-methylidene-1,3-propylenedisulfonic acid (IBDSA) in the reaction system are determined. When the IBSA concentration exceeds 12,000 mass ppm and/or the IBDSA concentration exceeds 6,000 mass ppm, then the concentration of sulfur trioxide in the reaction system is reduced. Thus, ATBS having an IBSA content of 100 mass ppm or lower and an IBDSA content of 100 mass ppm or lower is produced.
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Page/Page column 9-10
(2010/12/26)
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- SYNTHESIS OF 2-ACRYLAMIDO-2-METHYLPROPANESULFONIC ACID - A NEW MONOMER FOR WATER-SOLUBLE POLYMERS
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The results are presented of synthesis of 2-acrylamido-2-methylpropanesulfonic acid from acrylonitrile and 2-methylpropene in the presence of oleum.The conditions for synthesis and isolation of the desired product have been optimized.The main product and by-products have been identified.
- Khalistova, I. D.,Podgornova, V. A.
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p. 1185 - 1188
(2007/10/02)
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- THERMOCHEMISTRY OF 2-ACRYLAMIDO-2-METHYLPROPANE-1-SULPHONIC ACID SYNTHESIS
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The caloric effect of 2-acrylamido-2-methylpropane-1-sulphonic acid synthesis was determined using an adiabatic calorimeter with isothermal mantle and a thermistor as temperature sensor. The monomer synthesis was realised by reaction between acrylonitrile (AN), isobutylene (IB) and oleum, according to the two schemes of reaction: (I) (AN + IB) + oleum, (II) (AN + oleum) + IB. The experimental results pointed out that, for both reaction schemes, the total caloric effect increases with the SO3 content in oleum. Also, the total caloric effect did not depend on the reagent mixing order for low SO3 percent concentration, but conversely, it depends on the reaction scheme when 16 percent SO3 oleum was used.
- Aelenei, Nicolae,Beldie, Camelia
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p. 1075 - 1082
(2007/10/03)
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