CN1631519A - Method for preparing hydrosulfide group cellulose modifying material - Google Patents
Method for preparing hydrosulfide group cellulose modifying material Download PDFInfo
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- CN1631519A CN1631519A CN 200410084394 CN200410084394A CN1631519A CN 1631519 A CN1631519 A CN 1631519A CN 200410084394 CN200410084394 CN 200410084394 CN 200410084394 A CN200410084394 A CN 200410084394A CN 1631519 A CN1631519 A CN 1631519A
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Abstract
The invention offers a way to produce attaching material used to heavy metal in gathering and separating water environment. The craft includes making shuji cellulose solution, polishing the solid attaching material by shuji cellulose solution, washing and heating. The feature of the invention makes shuji cellulose solution first, and then polishes the solid attaching material by shuji cellulose solution; its advantage is shortening the time of making shuji attaching material.
Description
Technical field
The present invention relates to a kind of preparation method of hydrosulfide group cellulose modifying material.Specifically, relate to a kind of heavy metal ion in enrichment, the isolating environment water body that is applied to, with the preparation method of hydrosulfide group cellulose modifying solid adsorption material.
Background technology
Hydrosulfide group cellulose is applied to analytical chemistry, various trace elements in the water is carried out enrichment, separated the history that had more than 20 year, be characterized in and quantitatively adsorb heavy metal ion, can utilize different elutriants that coexistent metallic ion is separated from each other according to the combined intensity difference of different elements again.There is not the commercialization hydrosulfide group cellulose in the market, and synthetic hydrosulfide group cellulose 48-96 consuming time hour, make troubles to the user.
Summary of the invention
The purpose of this invention is to provide a kind of drawback that can overcome above-mentioned prior art, the fast preparation method of the solid adsorption material of using hydrosulfide group cellulose modifying that use properties is superior.
Technical scheme of the present invention is: adopt when the Mierocrystalline cellulose esterification solid-liquid biphasic reaction to change into single homogeneous reaction prior art, with enhance esterification speed greatly; Carboxylate solution is modified the solid adsorption material surface immediately without aftertreatment.
Embodiment
The object of the present invention is achieved like this:
Adding Thiovanic acid 30.0 grams, diacetyl oxide 60.8 grams, Glacial acetic acid 5.0 grams, the vitriol oil 0.2 gram in 500 milliliters of ground wide-necked bottles add after shaking up and take off cotton 4.0 grams of ester, gently press cotton that it is immersed in the solution fully with glass stick, cover tight bottleneck with the ground lid.Port grinding bottle is placed 50 ℃ of baking oven insulations 5 hours.Take out port grinding bottle and add 5 gram activated carbon (or molecular sieve) from baking oven, magnetic agitation places port grinding bottle 35 ℃ of baking oven insulations 30 minutes again after 5 minutes.From baking oven, take out port grinding bottle, with qualitative filter paper elimination liquid phase.Be neutral with distilled water drip washing solid until leacheate.Hydrosulfide group cellulose modifying material can use immediately, and is standby after also can drying in nearly 40 ℃ of baking ovens.
Realization the object of the invention further describes:
The present invention adopt high density cellulose activation solvent-diacetyl oxide, substitute aqueous acetic acid of the prior art with Glacial acetic acid, make cellulose dissolution become solution in reaction medium.Esterification is carried out in single liquid phase, and esterification speed is accelerated greatly, and the side chain of carboxylate distributes also more even.Adding a small amount of sulfuric acid in the reaction process can catalytic esterification and absorb the water molecules that esterification produces the esterification balance is moved to the resultant direction.Esterifying liquid is directly used in the solid adsorption material surface is modified without aftertreatment, helps hydrosulfide group cellulose equably to the infiltration and the absorption of porous material inside like this, and has simplified modification greatly.To Adsorption of Heavy Metal Ions (Cd through the gac of hydrosulfide group cellulose modifying
2+, Pb
2+, Cu
2+) and elution property test: add in 50 milliliters of drop-burettes with the gac of 1 gram hydrosulfide group cellulose modifying and constitute adsorption column, the neutral aqueous solution 1L that contains 5 μ g/L heavy metal ion is with the flow of the 10ml/min adsorption column of flowing through, and the concentration of heavy metal ion in the mensuration effluent liquid of back is finished in absorption.Adsorption column 0.4mol/L dilute hydrochloric acid 20ml leaching regeneration, the concentration of heavy metal ion in the mensuration leacheate.Experimental result: adsorption column has been held back the ion that tries more than 98%; 0.4mol/L dilute hydrochloric acid can be with the complete wash-out of examination ion.Experimental result shows that hydrosulfide group cellulose modifying material is similar to the hydrosulfide group cellulose performance, and heavy metal ion in the environment water is had good enrichment, separating power equally.
The invention provides a kind of preparation method of hydrosulfide group cellulose modifying material, the preparation method is easy, quick.The absorption of hydrosulfide group cellulose modifying material, elution property can satisfy analytical chemistry fully to enrichment of trace heavy metal ionic and separation requirement in the environment.
Claims (5)
1. the preparation method of hydrosulfide group cellulose modifying material, preparation is applied to heavy metal ion in enrichment, the isolating environment water body, with the preparation method of hydrosulfide group cellulose modifying solid adsorption material, it is characterized in that preparation technology is by the preparation of thioglycolic fibre cellulose solution, form the modification of solid adsorption material, the washing and the drying process of material with the thioglycolic fibre cellulose solution.
2. the preparation method of hydrosulfide group cellulose modifying material according to claim 1, its feature also are to have adopted a high proportion of diacetyl oxide in the preparation process of thioglycolic fibre cellulose solution, and the weight percent of solution composition (W%) is:
Cotton 2.0-6.0%
Thiovanic acid 25-35%
Diacetyl oxide 52.5-70.9%
Glacial acetic acid 2.0-6.0%
Sulfuric acid 0.1-0.5%
3. according to the preparation method of claim 1,2 described hydrosulfide group cellulose modifying materials, its feature is that also the preparation of thioglycolic fibre cellulose solution is under 40 ℃ of-60 ℃ of temperature, and reaction is 3-10 hour in encloses container.
4. according to the preparation method of claim 1,2,3 described hydrosulfide group cellulose modifying materials, it is that solid adsorption material is soaked in the thioglycolic fibre cellulose solution that its feature also is solid adsorption material is modified, and soaks 30 minutes under 30 ℃ of-40 ℃ of temperature.
5. according to the preparation method of claim 1,4 described hydrosulfide group cellulose modifying materials, its feature is also that described solid adsorption material can enumerate activated carbon, molecular sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410084394XA CN1315569C (en) | 2004-11-22 | 2004-11-22 | Method for preparing hydrosulfide group cellulose modifying material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410084394XA CN1315569C (en) | 2004-11-22 | 2004-11-22 | Method for preparing hydrosulfide group cellulose modifying material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1631519A true CN1631519A (en) | 2005-06-29 |
| CN1315569C CN1315569C (en) | 2007-05-16 |
Family
ID=34847335
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410084394XA Expired - Fee Related CN1315569C (en) | 2004-11-22 | 2004-11-22 | Method for preparing hydrosulfide group cellulose modifying material |
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| CN (1) | CN1315569C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102360659A (en) * | 2011-06-24 | 2012-02-22 | 中国科学院宁波材料技术与工程研究所 | Magnetic submicron composite core-shell particles, and preparation method and application thereof |
| CN101787654B (en) * | 2010-01-26 | 2012-03-21 | 浙江大学 | Preparation method of heavy metal ion enrichment cellulosic material |
| RU2471721C1 (en) * | 2011-07-05 | 2013-01-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Ивановский государственный химико-технологический университет" | Method of modifying cellulose-based sorbents |
| CN103071462A (en) * | 2013-02-28 | 2013-05-01 | 南京工业大学 | Modified peanut shell Hg(II) adsorbent, and preparation method and application thereof |
| CN104368316A (en) * | 2014-11-18 | 2015-02-25 | 辽宁大学 | Sulfydryl cellulose type straw adsorbent and preparation method thereof as well as recycling of noble metal silver |
| CN105107471A (en) * | 2015-09-14 | 2015-12-02 | 内蒙古农业大学 | Sulphydryl lignocellulose/montmorillonite composite heavy metal ion adsorbent and preparation and application thereof |
| CN105771902A (en) * | 2016-05-27 | 2016-07-20 | 北京三聚环保新材料股份有限公司 | Preparation method and application of sulfhydryl activated carbon mercury removal agent |
| CN109060792A (en) * | 2018-09-07 | 2018-12-21 | 天津市光复科技发展有限公司 | The method of sulfhydryl paper concentration and separation colorimetric method for determining trace lead in water |
| CN109239060A (en) * | 2018-09-07 | 2019-01-18 | 天津市光复科技发展有限公司 | The sulfhydryl paper enrichment of heavy metal cadmium, separation colorimetric method measuring method in water |
| CN111545178A (en) * | 2020-04-15 | 2020-08-18 | 济南大学 | Preparation method of biological adsorbent for separating sodium cyclamate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11174054A (en) * | 1997-12-08 | 1999-07-02 | Tadayuki Imanaka | Measuring method for heavy metal and recovery method therefor |
| CN1317445C (en) * | 2003-12-02 | 2007-05-23 | 中国科学院东北地理与农业生态研究所 | Method for preparing mercapto cotton |
-
2004
- 2004-11-22 CN CNB200410084394XA patent/CN1315569C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787654B (en) * | 2010-01-26 | 2012-03-21 | 浙江大学 | Preparation method of heavy metal ion enrichment cellulosic material |
| CN102360659A (en) * | 2011-06-24 | 2012-02-22 | 中国科学院宁波材料技术与工程研究所 | Magnetic submicron composite core-shell particles, and preparation method and application thereof |
| RU2471721C1 (en) * | 2011-07-05 | 2013-01-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Ивановский государственный химико-технологический университет" | Method of modifying cellulose-based sorbents |
| CN103071462A (en) * | 2013-02-28 | 2013-05-01 | 南京工业大学 | Modified peanut shell Hg(II) adsorbent, and preparation method and application thereof |
| CN104368316A (en) * | 2014-11-18 | 2015-02-25 | 辽宁大学 | Sulfydryl cellulose type straw adsorbent and preparation method thereof as well as recycling of noble metal silver |
| CN105107471A (en) * | 2015-09-14 | 2015-12-02 | 内蒙古农业大学 | Sulphydryl lignocellulose/montmorillonite composite heavy metal ion adsorbent and preparation and application thereof |
| CN105107471B (en) * | 2015-09-14 | 2017-12-29 | 内蒙古农业大学 | Sulfydryl lignocellulosic/montmorillonite Composite heavy metal absorbent and preparation and application |
| CN105771902A (en) * | 2016-05-27 | 2016-07-20 | 北京三聚环保新材料股份有限公司 | Preparation method and application of sulfhydryl activated carbon mercury removal agent |
| CN109060792A (en) * | 2018-09-07 | 2018-12-21 | 天津市光复科技发展有限公司 | The method of sulfhydryl paper concentration and separation colorimetric method for determining trace lead in water |
| CN109239060A (en) * | 2018-09-07 | 2019-01-18 | 天津市光复科技发展有限公司 | The sulfhydryl paper enrichment of heavy metal cadmium, separation colorimetric method measuring method in water |
| CN109060792B (en) * | 2018-09-07 | 2021-02-12 | 天津市光复科技发展有限公司 | Method for determining trace lead in water by sulfydryl paper enrichment and separation colorimetric method |
| CN111545178A (en) * | 2020-04-15 | 2020-08-18 | 济南大学 | Preparation method of biological adsorbent for separating sodium cyclamate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1315569C (en) | 2007-05-16 |
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Granted publication date: 20070516 |