CN1580087A - Preparation of high-water-absorption material from sa-son seed gum graft polymeric acrylic acid (salt) by microwave radiation - Google Patents

Preparation of high-water-absorption material from sa-son seed gum graft polymeric acrylic acid (salt) by microwave radiation Download PDF

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Publication number
CN1580087A
CN1580087A CN 03134533 CN03134533A CN1580087A CN 1580087 A CN1580087 A CN 1580087A CN 03134533 CN03134533 CN 03134533 CN 03134533 A CN03134533 A CN 03134533A CN 1580087 A CN1580087 A CN 1580087A
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China
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water
microwave radiation
salt
acrylic acid
preparation
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CN 03134533
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CN1239539C (en
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王云普
张继
袁昆
王永峰
李玉峰
刘小军
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Northwest Normal University
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Northwest Normal University
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Abstract

This invention refers to a kind of method of producing sopping material by grafting sand sagebrush gum into crylic acid (acrylate) in microwave radiation. The manufacturing engineering is to neutralize the crylic acid partially with sodium hydroxide, potassium hydroxide or ammonia, then adds initiator and sand sagebrush gum or other vegetable gum to it when whisking and puts it into microwave response operator after the system is well-proportioned. You should adjust it to certain radiation power and radiation time, without adding crosslinking agent to it, to graft the sand sagebrush gum into crylic acid and dry the product. After smashed, it becomes the final product. The water absorption rate of the sopping material produced by the invention is between 400ml/s and 500ml/s. The polyreaction only needs between 4min and 5min after adopting the microwave radiation technology. This invention can solve the problem of high cost of now-existing sopping material. The product can be used as anti wind erosion agent and sand-fixation agent in the field of entironment and play an active role in advancing germination, anti-drought and other dry farming.

Description

With microwave radiation artemisia glue graft polymerization vinylformic acid (salt) preparation high-absorbent material
Technical field
The present invention relates to a kind of water-absorbing material, particularly use the water-absorbing material of microwave radiation artemisia glue graft acrylic acid (salt) preparation.
Technical background
Microwave has stepped into chemical field gradually as a kind of brand-new energy, and it just more and more is subjected to people's attention to the promoter action of chemical reaction.Microwave is used for synthetic chemistry and starts from R.GEDGE in 1986 etc. and use the microwave esterification, hydrolysis, and after this research of oxidation and nucleophilic substitution and DIELS-ALDER cycloaddition reaction, all obtained very big success in tens class building-up reactionss of organic compound.In addition, microwave is at analytical chemistry, polyreaction, chemical engineering, existing many application the in aspects such as metallic ore smelting.Studies show that in recent years, microwave radiation can make some polysaccharose substances that special reaction takes place.
Sand sagebrush (Artemisia filifolia) (Artemisia desertorum), perennial grass undergraduate course plant extensively distributes, grows in hillside, mountain valley and the desert region of high altitude localitiess such as China northeast, North China and northwest, has maintenance soil, fixes the sand the effect of sand prevention.Its seed is a chocolate, is about 1mm, and the fruit of smooth oval shape contains a large amount of artemisia glue in the fruit.Artemisia glue is a kind of poly-mixed polysaccharide that may have crosslinking structure.It is different from starch, Mierocrystalline cellulose etc., and its viscosity is equivalent to 800 times of gelatin, itself can absorb 60 times water, and chemical property is stable.Required time of its conventional graft reaction is long, and grafting efficiency is low.The present invention utilizes and separate the poly-polysaccharide of sand sagebrush (Artemisia filifolia) from the industrial residue after the oil expression of sand sagebrush (Artemisia filifolia) seed, carries out graft polymerization with vinylformic acid under microwave radiation, prepares novel water-absorbing material.The present invention is based on wild sand sagebrush (Artemisia filifolia) and belong to per nnial herb, sand sagebrush (Artemisia filifolia) seed reserves are abundant, and plant resources can constantly be regenerated; Next water-absorbing material that makes is used to improve soil, and cost is lower when administering Desertification, can reach the purpose with " sand " sand control.
Summary of the invention
The purpose of this invention is to provide a kind ofly, prepare a kind of novel cheaply water-absorbing material, make it can be, fix the sand kind of a careless aspects to be applied in improvement of the ecological environment through microwave radiation polymerization with vinylformic acid (salt) grafting artemisia glue or other vegetable jelly.
Purpose of the present invention can realize by following measure:
A kind of with microwave radiation artemisia glue graft acrylic acid (salt) preparation water-absorbing material, under the ice-water bath cooling, with in the sodium hydroxide and vinylformic acid, and add initiator in the acrylate after neutralization, fully stir, make it evenly after, slowly add artemisia glue, carry out vigorous stirring, monomer and initiator are evenly spread in the sand sagebrush (Artemisia filifolia) colloid, obtain the pre-reaction thing.The pre-reaction thing is placed the microwave reaction device.The conciliation radiation power is 180w, and radiated time is 4min, carries out artemisia glue grafted propylene hydrochlorate polyreaction.After the reaction, take out product, put into drying plant,, pulverize, pack 60-70 ℃ of oven dry down.
Artemisia glue: vinylformic acid: the part between sodium hydroxide (the solution quality ratio is 18%) is than being 1: 5: 10.
With in the vinylformic acid and can also be potassium hydroxide or ammoniacal liquor.
The graft polymerization of preparation vinylformic acid (salt) can also be Viscogum BE or guar gum or tamarind seed gum.
The present invention compared with prior art has following advantage:
1, the present invention makes shorten greatly than popular response reaction time owing to used microwave technology, and energy consumption is low, and the product water absorbing properties that obtains is good, and it is according to seeing Table 1
Table 1
Reaction times Water-intake rate (ml/g)
Popular response Microwave radiation Popular response Microwave radiation
????6-7h ????4min ??300-400 ????400-500
2, the water-absorbing material of gained of the present invention---graft polymerization product, its percentage of grafting are 56%, and grafting efficiency is up to 94%, and monomer conversion reaches 99%.
3, the industrial residue of the present invention after with the wild sand sagebrush (Artemisia filifolia) seed oil expression of cheapness is raw material, through microwave radiation synthesizing new water-absorbing material, its cost only for 50% of existing water-holding agent, helps in improvement of the ecological environment, and drought resisting is fixed the sand kind of a careless tree planting aspects and obtained large-scale popularization and use.
4, utilize other vegetable jelly of prepared vinylformic acid of the present invention (salt) graft polymerization, can prepare water-absorbing material equally.What table 2 characterized is the water absorbing properties of the various vegetable jelly gained of microwave radiation vinylformic acid (salt) graft polymerization water-absorbing material.
Table 2
The vegetable jelly title Artemisia glue Viscogum BE Guar gum Tamarind seed gum
The product water absorbent rate ????450-500 ??400-450 ??350-400 ??360-400
Inhale the physiological saline rate ????34-35 ??50-55 ??48-50 ??50-53
5, utilize the industrial residue after the oil expression of sand sagebrush (Artemisia filifolia) seed to help environmental protection, and this technology itself do not produce industry " three wastes " in process of production, meet the industry policy of country for raw material.
When 6, the present invention prepares water-absorbing material, need not to use linking agent to carry out chemically crosslinked.
7, technical process of the present invention is short, stable, reliable.
Embodiment
The present invention also will be described in further detail in conjunction with the embodiments:
Embodiment one:
Under ice-water bath cooling, 5 parts of vinylformic acid are neutralized with 18% sodium hydroxide, to degree of neutralization be 80%.Add 0.1 part of initiator (0.1g/ml) again, fully stir the artemisia glue that adds 1 part down.After stirring, place the microwave reaction device, the adjusting radiation power is 180W, and radiated time 4min carries out graft polymerization.After reaction is finished, product is put into 65 ℃ of equipment dry, pulverize then, measure performances such as its water-intake rate.With product in apparatus,Soxhlet's with behind the acetone extraction 36h, calculate its grafting efficiency, percentage of grafting and monomer conversion etc.And use infrared spectra (FT-IR), scanning electron microscope (TEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TG-DTA) etc. and characterize.
Embodiment two:
Under ice-water bath cooling, 5 parts of vinylformic acid are neutralized with 18% potassium hydroxide, to degree of neutralization be 80%.Add 0.1 part of initiator (0.1g/ml) again, fully stir the Viscogum BE that adds 1 part down.After stirring, place the microwave reaction device, the adjusting radiation power is 180W, and radiated time 4min carries out graft polymerization.After reaction is finished, product is put into 68 ℃ of equipment dry, pulverize then, measure performances such as its water-intake rate.With product in apparatus,Soxhlet's with behind the acetone extraction 36h, calculate its grafting efficiency, percentage of grafting and monomer conversion etc., and use infrared spectra (FT-IR), scanning electron microscope (TEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TG-DTA) etc. and characterize.
Embodiment three:
Under ice-water bath cooling, 5 parts of vinylformic acid are neutralized with 18% ammoniacal liquor, to degree of neutralization be 80%.Add 0.1 part of initiator (0.1g/ml) again, fully stir the guar gum that adds 1 part down.After stirring, place the microwave reaction device, the adjusting radiation power is 180W, and radiated time 4min carries out graft polymerization.After reaction is finished, product is put into 70 ℃ of equipment dry, pulverize then, measure performances such as its water-intake rate.With product in apparatus,Soxhlet's with behind the acetone extraction 40h, calculate its grafting efficiency, percentage of grafting and monomer conversion etc., and use infrared spectra (FT-IR), scanning electron microscope (TEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TG-DTA) etc. and characterize.
Embodiment four:
Under ice-water bath cooling, 5 parts of vinylformic acid are neutralized with 18% sodium hydroxide, to degree of neutralization be 80%.Add 0.1 part of initiator (0.1g/ml) again, fully stir the tamarind seed gum that adds 1 part down.After stirring, place the microwave reaction device, the adjusting radiation power is 180W, and radiated time 4min carries out graft polymerization.After reaction is finished, product is put into 60 ℃ of equipment dry, pulverize then, measure performances such as its water-intake rate.With product in apparatus,Soxhlet's with behind the acetone extraction 40h, calculate its grafting efficiency, percentage of grafting and monomer conversion etc., and use infrared spectra (FT-IR), scanning electron microscope (TEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TG-DTA) etc. and characterize.

Claims (5)

1, a kind of with microwave radiation artemisia glue graft acrylic acid (salt) preparation water-absorbing material, it is characterized in that: under the ice-water bath cooling, with in the sodium hydroxide and vinylformic acid, and the adding initiator, fully stir, make it evenly after, slowly add artemisia glue, stir fast, monomer and initiator are evenly spread in the sand sagebrush (Artemisia filifolia) colloid, obtain the pre-reaction thing.The pre-reaction thing is placed the microwave reaction device, carry out the microwave radiation graft polymerization reaction, after the reaction, take out product,, pulverize, pack 60-70 ℃ of oven dry down.
2, according to the described a kind of water-absorbing material with microwave radiation artemisia glue graft acrylic acid (salt) polymerization preparation of claim 1, it is characterized in that artemisia glue: vinylformic acid: the part between sodium hydroxide (massfraction is 18%) is than being 1: 5: 10.
3, according to the described a kind of water-absorbing material with microwave radiation artemisia glue graft acrylic acid (salt) polymerization preparation of claim 1, it is characterized in that reconciling radiation power is 180w, and radiated time is 4min, carries out graft polymerization reaction.
4, according to claim 1 or 2 described a kind of water-absorbing materials with microwave radiation artemisia glue graft acrylic acid (salt) polymerizations preparation, it is characterized in that with vinylformic acid in and can also be potassium hydroxide or ammoniacal liquor.
5, according to claim 1 or 2 described a kind of water-absorbing materials with microwave radiation artemisia glue graft acrylic acid (salt) polymerization preparation, it is characterized in that preparing vinylformic acid (salt) graftomer can also be Viscogum BE, guar gum or tamarind seed gum.
CN 03134533 2003-08-14 2003-08-14 Preparation of high-water-absorption material from sa-son seed gum graft polymeric acrylic acid (salt) by microwave radiation Expired - Fee Related CN1239539C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101982504A (en) * 2010-10-11 2011-03-02 内蒙古大学 Method for preparing plate by utilizing polyacrylic acid and sodium salt thereof as adhesive and waste plant fiber
CN106317331A (en) * 2015-06-19 2017-01-11 上海东升新材料有限公司 Method for preparing butyl acrylate grafted guar gum by microwave radiation
CN110079331A (en) * 2019-03-28 2019-08-02 内蒙古自治区林业科学研究院 A kind of preparation of water-soluble environment protective sand-consolidating agent and application method
CN114478848A (en) * 2021-12-28 2022-05-13 中化泉州石化有限公司 Method for purifying and decontaminating polyolefin graft

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101982504A (en) * 2010-10-11 2011-03-02 内蒙古大学 Method for preparing plate by utilizing polyacrylic acid and sodium salt thereof as adhesive and waste plant fiber
CN101982504B (en) * 2010-10-11 2011-11-02 内蒙古大学 Method for preparing plate by utilizing polyacrylic acid and sodium salt thereof as adhesive and waste plant fiber
CN106317331A (en) * 2015-06-19 2017-01-11 上海东升新材料有限公司 Method for preparing butyl acrylate grafted guar gum by microwave radiation
CN110079331A (en) * 2019-03-28 2019-08-02 内蒙古自治区林业科学研究院 A kind of preparation of water-soluble environment protective sand-consolidating agent and application method
CN110079331B (en) * 2019-03-28 2021-04-06 内蒙古自治区林业科学研究院 Preparation and application method of water-soluble environment-friendly sand fixing agent
CN114478848A (en) * 2021-12-28 2022-05-13 中化泉州石化有限公司 Method for purifying and decontaminating polyolefin graft
CN114478848B (en) * 2021-12-28 2023-06-30 中化泉州石化有限公司 Method for purifying and removing impurities of polyolefin graft

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