SU1645308A1 - Method of solution preparation for fibres moulding - Google Patents

Abstract

The invention relates to the field of chemical technology, specifically to the preparation of solutions of cellulose in N-methylmoroline-M-oxide, suitable for the preparation of hydrated cellulose fibers and films. The invention allows the process to grow and reduce the destruction of cellulose due to the fact that cellulose is mixed with N-methylmorlolene-N-oxide hydrate, containing 6-10 wt.% Water with a mass ratio of cellulose and hydrate M-methylmor- (N-N oxide 15-35: 65-85 at room temperature until the mixture is completely homogenized and its melting temperature reaches 105-135 ° C. 1 tab. $ (L s

Description

The invention relates to chemical technology, in particular, to methods for preparing solutions of cellulose in N-methylmorvyulin-N-oxide (MMO) suitable for producing hydrated cellulose fibers and films.

The purpose of the invention is to simplify the process and reduce the destruction of cellulose.

Example 1. To prepare a 15% cellulose solution, vibromills in the working unit are loaded with cellulose (n) 15 / of the total mass and MMO hydrates, contents 10 MW:% of water, m.p. 120 ° C). Cellulose is used; degree of polymerization is 700. The initial heterogeneous mixture is subjected to joint processing on a vibromill for 4 minutes at a SO Hz processing frequency. conditions of room temperature. Getting homogenous

the powdered reaction mixture has a mp. 105 ° C When heated in a heated thermostatically controlled head at 105 ° C, the mixture melts, forming a clear solution within 1 minute. Studies conducted with a polarization microscope show that the resulting solution has a high degree of homogeneity. The degree of polymerization of cellulose in the resulting solution is 600. The physicomechanical properties of the hydrated cellulose fibers obtained are as follows. These are: a breaking strength of 32.2 cN / tex, a breaking elongation of 12.1%, the values given are at the level of viscose fibers.

PRI mme R 2. Preparation of the solution of cellulose is carried out as in example 1, with the content in the mixture of cellulose in the amount of 18 wt.% And hydrate

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MO, containing 10 wt.% Of water, during the treatment in the heterophase until the mixture is homogeneous is min, and so pl. the resulting mixture rava 110 ° C. The subsequent melting of the mixture is carried out at 10 ° C for 3 minutes. The resulting clear solution is characterized by high homogeneity, the polymerization temperature of cellulose is 600. The physical and mechanical properties of the molded fibers are similar to those shown in Example 1.

Example 3. The preparation of the cellulose solution is carried out as ke, as in jc and in example 1, with 35 wt.% And (MO, containing 10 May. 7 water) in a mixture of cellulose. The mixing is carried out in a screw mixer with mechanical force on the shaft 2p of the screw, equal to 5 kgf "m, for 1 Omin until a homogeneous mixture is obtained. The strain of the mixture obtained is 115. The subsequent melting of the mixture is carried out at 115 ° C for 4 minutes. The resulting solution is characterized high homogeneity, degree of polymerization of cellulose 480, physicomechanical properties windows are at a level of fiber properties "

example 1j

EXAMPLE 4 The preparation of the cellulose solution is carried out in the same way as in example 1, with a content in the mixture of cellulose in an amount of 15% by weight and an MMO hydrate containing 8% by weight of water Tpsl. I,, the processing time in the heterophase is 3 min before the formation of a homogeneous mixture, m.p. the resulting mixture is 125 ° C; Follow-. p

40

melting, see, and carried out at 1-25 ° C for 1 min. The solution obtained is lysokohomogenic, the degree of polymerization of celium is 650. The physicochemical properties of the molded fibers are at the level of the properties of the fibers according to

example i

Example 5 The preparation of the cellulose solution is carried out as in Example 1, with a mixture of cellulose in an amount of 20% by weight and MMO hydrate with 8% by weight of water. The processing time is 5 minutes, so that. the resulting mixture is 125 ° C. When the mixture is melted at 125 ° C for 2 minutes, a homogeneous plant is formed - 5% Cp, the degree of polymerization of cellulose is 600. The properties of the fibers are similar to those of the fibers of Example 1.

EXAMPLE 6 The preparation of the cellulose solution was carried out as in Example 3, with a content of 35% by weight of cellulose and an MMO hydrate with 8% by weight of water in the mixture. The processing time in the mecic mixer is 8 minutes, so pl. the resulting mixture 130 ° C. Melting the mixture at 130 ° C leads to the formation of a homogeneous solution, the degree of polymerization of cellulose 500. The properties of the fibers are similar to the properties of fibers in example I.

Example. The preparation of the cellulose solution was carried out as in Example 1, with the content in the mixture of cellulose in an amount of 15 wt.% And MMO hydrate with 6 wt.% Of water, mp, 150 ° C, treatment time, 3 min, mp . the resulting mixture is 135 ° C. When the mixture is melted at I35 ° C for a minute, a homogeneous solution is formed, the degree of polymerization of cellulose is 570. The properties of the fibers are similar to those of the fibers of example 1.

PRI me R 8. Preparation of the cellulose solution is carried out as in Example 1, with a content of 20% by weight of cellulose and MMO hydrate with 6% by weight of water, the activation time in the heterophase is equal to 5 min, mp. the resulting mixture 125 ° C. Upon subsequent heating at I25 C, the mixture melts to form a homogeneous solution, the degree of polymerization of cellulose is 600, the properties of the fibers are similar to those of the fibers of example I

Nimer9. The preparation of the cellulose solution was carried out in the same way as in example 3, with the content in the mixture of cellulose in an amount of 35 wt.% And MMO with b wt.% Of water, activation processing for 6 minutes results in a mixture with mp 125 ° s Melting the mixture for 3 minutes leads to the formation of a homogeneous solution, the degree of polymerization of cellulose 500. The properties of the fibers are similar to those of the fibers of example 1.

PRI me R 10 (comparative /. The preparation of the cellulose solution is carried out in the same manner as in example H, when the content in the mixture is cellulose in an amount of 37% by weight. The powder mixture does not melt at 125 ° C. 140 C is not completely melted. The subsequent melting of the mixture leads to the formation of a heterogeneous solution with undissolved cellulose particles.

Example 11 (comparative). The preparation of the cellulose solution is carried out as in Example 2, the treatment time in heteroAase is 15 minutes, m.p. the mixture obtained is 100 ° C. When the mixture is melted, a homogeneous solution is formed, the degree of polymerization of cellulose is 400.

Example 12 (comparative). The preparation of the cellulose solution was carried out as in Example 7, with a treatment time of 1 minute. Get a mixture with so pl, 140 ° C. When the mixture is melted at 140 ° C, the solution darkens very quickly, active decomposition processes take place, and the degree of polymerization of cellulose is 380.

Data on the proposed method in comparison with the known are presented in the table.

Claims (1)

Invention Formula A method for producing a fiber spinning solution, comprising a blending-. cellulose with N-methylmorpholine-01-oxide hydrate containing water, characterized in that 53086 To simplify the process and reduce the destruction of cellulose, N-methylmorlolene-N-oxide hydrate is used, containing 6-10% by weight of water, and mixing is carried out at a mass ratio of cellulose and N-methylmorpholine-M-oxydate 15-35: 65-85, respectively, at room temperature until the mixture is completely homogenized and its melting temperature reaches 105-135 ° C. five The method of obtaining a solution of cellulose Number of technological stats The degree of polymerization of cellulose in solution Famous Proposed 4 (mixing pulp with MMO, mixing, distilling water, vacuuming) 1 (mixing for 1-8 minutes) 280-420 480-560