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Cross-linked shperical macroporous cellulose bead and clean preparing process by jetting method

A technology of cellulose and jetting method, which is applied to the preparation of macroporous cross-linked spherical cellulose beads by jetting and its cleaning process and the recovery of solvents, can solve the problem of restricting the development of spherical cellulose adsorbents, environmental pollution, and inability to use For the preparation of cellulose beads and other issues, to broaden the development approach, reduce production costs, and improve the effect of added value

Inactive Publication Date: 2005-12-28
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvents currently used to dissolve cellulose are mainly copper ammonia complex solvents, cadmium ethylenediamine complex solvents and PF / DMSO, N 2 o 4 / DMSO, L NH 3 / NH 4 Solvents such as SCN and LiCl / DMAc, because some solvents are still in the experimental stage, and some have the possibility of realizing production, but they cannot be used as raw material solutions for the preparation of cellulose beads, so many domestic and foreign researchers choose Inexpensive and convenient source of viscose to prepare cellulose beads [1-8]
However, a large amount of waste liquid (such as waste lye, etc.), waste gas (such as CS 2 、H 2 S, SO 2 and other harmful gases) and waste (such as solid waste, etc.), causing serious pollution to the environment, and to a certain extent restricting the development of spherical cellulose adsorbents

Method used

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  • Cross-linked shperical macroporous cellulose bead and clean preparing process by jetting method
  • Cross-linked shperical macroporous cellulose bead and clean preparing process by jetting method

Examples

Experimental program
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Embodiment 1

[0043] Embodiment 1: the process steps and order of the present embodiment are as figure 1 shown. Specific steps are as follows:

[0044] (1) dissolve

[0045] Raw materials and formula (unit-kilogram) of the present embodiment:

[0046] Cotton linters: 2.0 kg

[0047] NMMO·H 2 O: 95 kg

[0048] Stabilizer (mixture of oxalic acid and isoascorbic acid, mass ratio 4:1): 1 kg

[0049] Porogen (calcium carbonate): 2 kg

[0050] Dissolving process steps and process parameters: 2.0 kg of pulp or cotton is put into a reactor containing 95 kg of N-methylmorpholine-N-oxide (N-methylmorpholine-N-oxide, NMMO) aqueous solution, and the reaction temperature Controlled at 75°C, dissolved and reacted for 90 minutes to form a cellulose-NMMO-water solution with a mass fraction of 2.06%, then added 1 kg of a stabilizer of a mixture of oxalic acid and isoascorbic acid and 2 kg of a calcium carbonate porogen. This process step is carried out under normal pressure.

[0051] (2) Spraying, ...

Embodiment 2

[0062] Embodiment 2: the process steps and order of the present embodiment are as figure 1 shown. Specific steps are as follows:

[0063] (1) dissolve

[0064] Raw materials and formula (unit-kilogram) of the present embodiment:

[0065] Deinked waste paper pulp: 1.0 kg

[0066] NMMO·H 2 O: 97 kg

[0067] Stabilizer (mixture of oxalic acid and isoascorbic acid, mass ratio 7:1): 0.5 kg

[0068] Porogen (sodium carbonate): 1.5 kg

[0069] Dissolving process steps and process parameters: put the above-mentioned amount of pulp or cotton into the reactor containing the above-mentioned amount of N-methylmorpholine-N-oxide (N-methylmorpholine-N-oxide, NMMO for short) aqueous solution, and The reaction temperature was controlled at 65°C, and the dissolution reaction was carried out for 120 minutes to form a cellulose-NMMO-water solution with a mass fraction of 1.02%, and then the above-mentioned amount of stabilizer and porogen was added. This process step is carried out under...

Embodiment 3

[0081] Embodiment 3: the process steps and order of the present embodiment are as figure 1 shown. Specific steps are as follows:

[0082] (1) dissolve

[0083] Raw materials and formula (unit-kilogram) of the present embodiment:

[0084] Masson pine bleached pulp: 4.0 kg

[0085] NMMO·H 2 O: 91 kg

[0086] Stabilizer (methyl ethyl ketoxime and its mixture, mass ratio 32:1): 2.0 kg

[0087] Porogen (sodium bicarbonate): 3.0 kg

[0088] Dissolving process steps and process parameters: put the above-mentioned amount of pulp or cotton into the reactor containing the above-mentioned amount of N-methylmorpholine-N-oxide (N-methylmorpholine-N-oxide, NMMO for short) aqueous solution, and The reaction temperature was controlled at 85°C, and the dissolution reaction was carried out for 80 minutes to form a cellulose-NMMO-water solution with a mass fraction of 4.21%, and then the above-mentioned amount of stabilizer and porogen was added. This process step is carried out under no...

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Abstract

The invention discloses a macroporous cross-linked spherical cellulose bead and its cleaning spray method preparation process. The steps are as follows: dissolving pulp or cotton at a suitable temperature to form a cellulose-NMMO-water solution with a suitable mass fraction, and adding Stabilizer and porogen; at a suitable temperature, it is directly sprayed into the coagulation bath composed of NMMO aqueous solution and surfactant through an adjustable spray gun, cross-linked and solidified under stirring, and the specific surface area of ​​different particle sizes is 120-760m 2 / g, moisture content 50%-80%, skeleton density 0.86-1.28g / ml, apparent density 0.47-0.72g / ml, pore volume 0.23-1.06ml / g, pore size 80%-97% Linked spherical cellulose beads. The manufacturing process of the invention is simple and non-toxic. The product has good swelling resistance, oxidation resistance, biodegradation resistance and acid and alkali degradation resistance.

Description

Technical field: [0001] The invention belongs to the field of functional macromolecular materials, and in particular relates to the preparation of macroporous crosslinked spherical cellulose beads by spraying method, its cleaning process and the recovery method of solvent. Background technique: [0002] In today's world, the reserves of oil and natural gas resources are limited, and their research, development and utilization have an increasingly serious impact on the earth's ecological environment, which has prompted the vigorous development of polymer materials that use natural resources as raw materials. Cellulose is the most abundant and recoverable natural resource on the earth. It is cheap, degradable and does not pollute the environment. Therefore, all countries in the world attach great importance to the research and development of cellulose. Cellulose adsorbent is one of the important development directions of cellulose functional polymer materials. This kind of ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08L1/02
Inventor 刘明华叶莉黄建辉
Owner FUZHOU UNIV
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