CN103044295A - Method for purifying 2-methyl-2-acrylamido propanesulfonic acid - Google Patents

Method for purifying 2-methyl-2-acrylamido propanesulfonic acid Download PDF

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CN103044295A
CN103044295A CN 201110326280 CN201110326280A CN103044295A CN 103044295 A CN103044295 A CN 103044295A CN 201110326280 CN201110326280 CN 201110326280 CN 201110326280 A CN201110326280 A CN 201110326280A CN 103044295 A CN103044295 A CN 103044295A
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methyl
propanesulfonic acid
acrylamido propanesulfonic
purification
acrylamido
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何阳
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Abstract

The invention discloses a method for purifying 2-methyl-2-acrylamido propanesulfonic acid. The method comprises the following steps of: (a) firstly, weighing a certain amount of 2-methyl-2-acrylamido propanesulfonic acid solid powder, and putting the 2-methyl-2-acrylamido propanesulfonic acid solid powder into a reaction vessel; (b) then, dissolving the 2-methyl-2-acrylamido propanesulfonic acid solid powder to form a supersaturated solution; and (c) finally, performing suction filtration after stirring and fully dissolving, and drying the separated 2-methyl-2-acrylamido propanesulfonic acid crystals for later use. By adopting the method, the 2-methyl-2-acrylamido propanesulfonic acid can be quickly purified, the purification efficiency is high, the purification steps are simple, and the purification cost is greatly reduced.

Description

The method of purification of a kind of 2-methyl-2-acrylamido propanesulfonic acid
Technical field
The present invention relates to the method for purification of a kind of 2-methyl-2-acrylamido propanesulfonic acid.
Background technology
Thickening material is a kind of auxiliary rheological agents, not only can make the coating thickening, prevents from the sagging phenomenon occurring in the construction, and can give mechanical property and the package stability of coating excellence.For the lower water-borne coatings of viscosity, it is a very important analog assistant.
Available thickening material kind is a lot of in the market, mainly contains inorganic thickening agent, cellulose family, polyacrylic ester and association type polyurethane thickener four classes.The use history of cellulose thickener is long, kind is a lot, and methylcellulose gum, carboxymethyl cellulose, Natvosol, Vltra tears etc. are arranged, and once is the main flow of thickening material, and wherein the most frequently used is Natvosol.Polyacrylate thickeners can be divided into two kinds basically: a kind of is water miscible polyacrylate; Another kind is homopolymer or the copolymer emulsion thickening material of vinylformic acid, methacrylic acid, and this thickening material itself is acid, must just can reach thickening effectiveness with alkali or ammonia neutralization to pH8~9, is also referred to as propylene soda acid swelling thickening material.The polyurethanes thickening material is associative thickener newly developed in recent years.Inorganic thickening agent is a class water-swelling and form thixotropic gel mineral.Mainly contain wilkinite, attapulgite, pure aluminium silicate etc., wherein wilkinite is the most commonly used.
The thickening mechanism of cellulose thickener cellulose thickener is that hydrophobic main chain and ambient water molecule pass through hydrogen bond association, has improved the fluid volume of polymkeric substance itself, has reduced the space of Particle free activity, thereby has improved the system viscosity.Also can realize by the winding of molecular chain the raising of viscosity, showing as static and low the shearing has high viscosity, is low-viscosity under high-shear.This is that cellulose molecular chain is in state of disarray and makes system present high viscosity because when static state or low shearing speed; And when high shear rates, molecule parllel is made ordered arrangement in flow direction, is easy to mutual slip, so the system viscosity degradation.
Its thickening mechanism of agent for polyacrylic acid thickening is that thickening material is soluble in water, and by the same sex electrostatic repulsion of carboxylic acid ion, molecular chain is stretched to bar-shaped by spirrillum, thereby has improved the viscosity of water.It also forms reticulated structure by building bridge between emulsion particle and pigment in addition, has increased the viscosity of system.
Association type polyurethanes thickening material A.J.Reuvers has done detailed research to the thickening mechanism of association type polyurethanes thickening material.Introduced hydrophilic radical and hydrophobic grouping in the molecular structure of this class thickening material, made it present the character of certain tensio-active agent.When its concentration of aqueous solution surpasses a certain certain concentration, form micella, micella and polymer particle associate and form reticulated structure, and the system viscosity is increased.Several micellas of molecular band have on the other hand reduced the transport property of water molecules, and the water viscosity is also improved.This class thickening material not only exerts an influence to the rheological of coating, and and adjacent latex particle between exist and interact, if this effect is too strong, cause easily the latex layering.
The inorganic thickening agent wilkinite is a kind of layered silicate, expand to form flocculent substance after the suction, has good suspension and dispersiveness, is combined into colloid with an amount of water, can discharge charged corpuscle in water, increases the system viscosity.
The thickening efficiency of cellulose thickener cellulose thickener is high, especially to the thickening of water; Restriction to coating coating is few, is widely used; Spendable pH scope is large.But exist levelling property relatively poor, splash phenomena is more during roller coat, stability is bad, is subject to the shortcomings such as microbiological deterioration.Because it is low-viscosity, static and low the shearing high viscosity is arranged, so after coating was finished, viscosity increased sharply, and can prevent sagging, causes but then levelling property relatively poor under high-shear.There are some researches show that the relative molecular mass of thickening material increases, the splashing property of latex coating also increases.Cellulose thickener splashes so easily produce because relative molecular mass is very large.This type of thickening material is to reach thickening effectiveness by " fixedly water ", and pigment and latex particle are seldom adsorbed, and the volumetric expansion of thickening material is full of whole water, and the pigment that suspends and latex particle are extruded on one side, produce easily flocculation, thereby stability is not good.Owing to be natural polymer, be subject to microorganism attack.
The agent for polyacrylic acid thickening agent for polyacrylic acid thickening has stronger thickening property and levelling property preferably, and biologically stable is good, but responsive to the pH value, water tolerance is not good.
This associative structure of association type polyurethanes thickening material is damaged under the effect of shearing force, and viscosity reduces, and when shearing force disappearance viscosity can recover again, can prevent that the sagging phenomenon from appearring in construction process.
And its viscosity recovers to have certain hysteresis quality, is conducive to the levelling of filming.The relative molecular mass of polyurethane thickener (thousands of to tens thousand of) is more much lower than the relative molecular mass (hundreds thousand of to millions of) of front two class thickening materials, can not encourage and splash.The water-soluble of cellulose thickener height can affect the water tolerance of filming, but has simultaneously hydrophilic and hydrophobic grouping on the polyurethanes thickening material molecule, and hydrophobic grouping has stronger affinity with the matrix of filming, and can strengthen the water tolerance of filming.Because latex particle participated in association, can not produce flocculation, thereby can make and film smoothly, higher glossiness is arranged.The many performances of association type polyurethane thickener are better than other thickening material, but because its unique micelle thickening mechanism, thereby those components that affect micella will inevitably exert an influence to thickening property in the formulation for coating material.During with this type of thickening material, various factors be should take into full account on the impact of thickening properties, the used emulsion of coating, defoamer, dispersion agent, film coalescence aid etc. do not changed easily.
Inorganic thickening agent water-based bentonite thickener has the advantages such as thickening property is strong, thixotropy good, pH value wide accommodation, good stability.But because wilkinite is a kind of inorganic powder, light absorptive is good, can obviously reduce film coated surface gloss, plays the effect of similar matting agent.So, when in the light latex coating is arranged, using wilkinite, note controlling consumption.Nanotechnology has realized the nanometer of particles of inorganic material, has also given inorganic thickening agent some new performances.
Thickening material commonly used has ether of cellulose and derivatives class, association type alkali swelling thickening material and polyurethane thickener.(1) ether of cellulose and derivative thereof: ether of cellulose and derivatives class thickening material thereof mainly contain Natvosol, methyl hydroxyethylcellulose, Type 3U, methylhydroxypropylcellulose etc.The hydrophobically modified Mierocrystalline cellulose is to introduce a small amount of long-chain hydrophobic alkyl at the Mierocrystalline cellulose hydrophilic skeleton, thereby becomes associative thickener, and its thickening effectiveness can be suitable with the much bigger ether of cellulose thickening material kind of relative molecular mass.
Thickening material has specific rheological property, and resistance to acid is first elected propylene glycol alginate; Increase the first-selected guar gum of tonality; In solution pseudo-plasticity, the cold water solubleness the strongest be xanthan gum; The attached property of emulsification holder is best with gum arabic; Gelation agar be better than other glue but the gel transparency especially with carrageenin for very; Carrageenin also is being better than other glue aspect the newborn class stability.
Thickening material claims again jelling agent, claims again thickener or foodstuff glue when being used for food.It can improve system viscosity, makes system keep uniformly stable suspended state or milkiness state, or forms gel.Be widely used in food, coating, sizing agent, makeup, washing composition, printing and dyeing, rubber, medicine and other fields.Again in the pigment printing, by the paint-printing colour size that thickening material, water, tackiness agent and pigment printing paste form, shearforce under the effect of Printing Machinery power, occurs in printing paste again, the viscosity that makes printing paste again moment decrease; When shearforce disappears, return to again original high viscosity, make the textile printing clear-cut.This viscosity that occurs with the variation of shearforce changes, and mainly realizes by thickening material.During emulsion paint was made again, thickening material played many-sided coordinative role to the thickening of emulsion paint, the stable rheological property that reaches.Be used as protective colloid in the emulsion polymerization process again, improve the stability of emulsion; Again pigment, fillers dispersed stage, improve the viscosity of dispersed material and be beneficial to dispersion; Improve again paint stability and freeze-thaw resistance in the storage and transport process, prevent that pigment, filler from sinking to the bottom caking; Regulate again the emulsion paint viscosity in the construction, and be good thixotropy etc.In food, add the food thickener of some thousandths of, have gelling, film forming, water holding, suspension, emulsification, foam stabilization and the effect such as lubricated.Relative stability to color, structure and the food of fluidised form food or frozen glue food plays a very important role.
Thickening material belongs to hydrophilic macromolecular compounds mostly, by sources is divided into animal class, plant, mineral substance, synthetic class or semi-synthetic class.Can be divided into natural and synthetic two large classes in simple minute.Natural product great majority are to produce from the plant and the seaweeds that contain the polyose viscous substance, such as starch, pectin, agar, gelatin, marine alga fat, carrageenin, dextrin, tragacanth gum, polysaccharide element derivative etc.; Synthetics has the derivatived celluloses such as methylcellulose gum, carboxymethyl cellulose, starch derivative, casein food grade, sodium polyacrylate, polyoxyethylene, polyvinylpyrrolidone, polyvinyl alcohol, low-molecular polyethylene wax, polyacrylamide etc.
Commonly used thickening material and the thickening material of being used as emulsion stabilizer mainly contain Xylo-Mucine, Protanal Ester SD-LB, carrageenin, xanthan gum, pectin, guar gum, Viscogum BE etc. in the drink production.
Because the economic crisis impact is not that short-term can get warm again after a cold spell, the China's GDP speedup glides, and consumption confidence is not enough, and enterprise's cutting down expenses reduces cost, and the thickening material operated pressure increases, and the trend that supply exceed demand is inevitable.
Studies show that all the time, industrial concentration is low in China thickening material enterprise, lack economies of scale.In recent years, because the continuous aggravation of market competition, the merging and reorganization between enterprise and brand operation process are progressively accelerated, and appropriate scale of operation wins initial success.The chain Main Patterns as appropriate scale of operation of grouping of the world economy and brand is enlarging and stable traveller, is improving consumer loyalty degree, reduces the aspects such as cost larger advantage is arranged.
Thickening material development is faced with new challenges, and the thickening material operation still need to recover in addition time, and the thickening material investment is considered to generally be tending towards saturated under the impact of financial crisis, and tired attitude has been displayed in the development of thickening material for the first time.Following investment wish returns rational, perhaps needs directional steering two or three line cities.The direction of following investment mainly is two or three line cities.The thickening material market in Some Domestic two or three line cities has possessed the condition that the investor encloses the land.
The development in China thickening material market temporarily also is faced with a lot of problems, but what be worth happiness is that increasing enterprise has had realized that great potential and the wide development prospect that thickening material market has, its future developing trend has also been reached comparatively unified understanding, believed and to bring larger life and vigor to whole thickening material market.
Chinese thickening material industry analysis investment landscape prediction address in 2011 is on a large amount of careful market study bases, Main Basis State Statistics Bureau, National Development and Reform Committee, Development Research Center of the State Council, national Department of Commerce, General Administration of China Customs, relevant industries association, announcements such as the Back ground Information of multiple relevant newspapers and periodicals and professional research unit both at home and abroad, provide a large amount of substantial in content, add up accurate data and data.Be based on current economic overall development situation; development situation and prospect, market competition structure and enterprise, investment strategy and Risk-warning, development trend and Management Suggestions etc. to rear crisis epoch China-styled Certain Industry Field are furtherd investigate, and selective analysis prospect and the risk of thickening material industry.Report has disclosed thickening material potential market demand and potential chance, provides the accurately decision-making foundation of market intelligence information and science for the Strategic Investor selects appropriate investment opportunity and company leader's layer to do strategic planning.
2-methyl-2-acrylamido propanesulfonic acid is as the reaction monomers of synthetic acid solution thickening material, and is higher to the monomer purity requirement at copolymerization, so need purify to the monomer of soon participating in reaction before reacting.The purpose of purifying is to remove stopper and some the impurity monomers that are mixed with in the starting monomer, in order to avoid because the existence of these impurity exerts an adverse impact to polyreaction, make polymerization product not reach expected effect.
Summary of the invention
The object of the invention is to overcome the shortcoming and defect of above-mentioned prior art, the method of purification of a kind of 2-methyl-2-acrylamido propanesulfonic acid is provided, this method of purification can be purified to 2-methyl-2-acrylamido propanesulfonic acid fast, and purification efficiency is high, purification step is simple, greatly reduces cost for purification.
Purpose of the present invention is achieved through the following technical solutions: the method for purification of a kind of 2-methyl-2-acrylamido propanesulfonic acid may further comprise the steps:
(a) at first, take by weighing a certain amount of 2-methyl-2-acrylamido propanesulfonic acid pressed powder and place reaction vessel;
(b) then, then dissolve 2-methyl-2-acrylamido propanesulfonic acid pressed powder, make it form supersaturated solution;
(c) last, through stirring, fully carry out suction filtration after the dissolving, with the 2-methyl of separating out-2-acrylamido propanesulfonic acid crystal dry for standby.
In the described step (a), reaction vessel is the Büchner funnel that is covered with filter paper.
In the described step (b), respectively with vinyl cyanide and methylene dichloride dissolving 2-methyl-2-acrylamido propanesulfonic acid pressed powder.
In the described step (c), dry by vacuum drier.
In sum, the invention has the beneficial effects as follows: can purify to 2-methyl-2-acrylamido propanesulfonic acid fast, and purification efficiency is high, purification step is simple, greatly reduces cost for purification.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited only to this.
Embodiment:
The method of purification of a kind of 2-methyl that the present invention relates to-2-acrylamido propanesulfonic acid, its concrete steps are as follows:
(a) at first, take by weighing a certain amount of 2-methyl-2-acrylamido propanesulfonic acid pressed powder and place reaction vessel;
(b) then, then dissolve 2-methyl-2-acrylamido propanesulfonic acid pressed powder, make it form supersaturated solution;
(c) last, through stirring, fully carry out suction filtration after the dissolving, with the 2-methyl of separating out-2-acrylamido propanesulfonic acid crystal dry for standby.
In the described step (a), reaction vessel is the Büchner funnel that is covered with filter paper.
In the described step (b), respectively with vinyl cyanide and methylene dichloride dissolving 2-methyl-2-acrylamido propanesulfonic acid pressed powder.
In the described step (c), dry by vacuum drier.
Above-mentioned method of purification can be purified to 2-methyl-2-acrylamido propanesulfonic acid fast, and purification efficiency is high, and purification step is simple, greatly reduces cost for purification.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction, and every foundation technical spirit of the present invention, any simple modification, equivalent variations to above embodiment does all fall within protection scope of the present invention.

Claims (4)

1. the method for purification of 2-methyl-2-acrylamido propanesulfonic acid is characterized in that, may further comprise the steps:
(a) at first, take by weighing a certain amount of 2-methyl-2-acrylamido propanesulfonic acid pressed powder and place reaction vessel;
(b) then, then dissolve 2-methyl-2-acrylamido propanesulfonic acid pressed powder, make it form supersaturated solution;
(c) last, through stirring, fully carry out suction filtration after the dissolving, with the 2-methyl of separating out-2-acrylamido propanesulfonic acid crystal dry for standby.
2. the method for purification of a kind of 2-methyl according to claim 1-2-acrylamido propanesulfonic acid is characterized in that, in the described step (a), reaction vessel is the Büchner funnel that is covered with filter paper.
3. the method for purification of a kind of 2-methyl according to claim 1-2-acrylamido propanesulfonic acid is characterized in that, in the described step (b), respectively with vinyl cyanide and methylene dichloride dissolving 2-methyl-2-acrylamido propanesulfonic acid pressed powder.
4. the method for purification of a kind of 2-methyl according to claim 1-2-acrylamido propanesulfonic acid is characterized in that, in the described step (c), dries by vacuum drier.
CN 201110326280 2011-10-13 2011-10-13 Method for purifying 2-methyl-2-acrylamido propanesulfonic acid Pending CN103044295A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014194690A1 (en) * 2013-06-06 2014-12-11 梅龙毅 Method for purifying acrylamide alkyl sulfonic acid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014194690A1 (en) * 2013-06-06 2014-12-11 梅龙毅 Method for purifying acrylamide alkyl sulfonic acid
US9745260B2 (en) 2013-06-06 2017-08-29 Longyi MEI Method for purifying acrylamide alkyl sulfonic acid

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Application publication date: 20130417