SU1427011A1 - Method of recovery of n-methylmorpholin-n-oxide from process solutions of hydrate cellulose fibre production - Google Patents

Description

(21) 3944738 / 23-05

(22) 08/19/85

(46) 09/30/88. Bksh. 36 (72) V.V.Smolikov, I.Z.Eyfer, S.P. Papkov, V.G.Kulichikhin, Yu, I, Belousov, I.P. Bashkeev and Finger

(53) 676.08 (088.8)

(56) Högert H.L. New methods for producing regenerated cellulose fibers. - Papier 1979, Ig 33, n. 12. S 562-568.

(54) METHOD FOR THE REGENERATION OF N-METHYLMORPHO- JMH-N-OKCKOA FROM TECHNOLOGICAL SOLUTIONS IN THE PRODUCTION OF NNDRATSELYULLOZO Fibers

(57) The invention relates to the production of chemical fibers, filaments and films, in particular to the production of fibers from cellulose solutions in direct

solvent K-methylmorpholine-M-oxyde by wet and dry-wet molding. The invention allows to completely (100%) regenerate N-methyl-morpholinoxide (MMO), used in the preparation of the spinning solution, due to the fact that spent technological solutions with an MMO concentration of 0.25-0.62% are passed through cationite, from which ammonia in a mixture of water and isopropyl alcohol at a mass ratio of ammonia, water and alcohol 1: (3-5) :( 14-16) remove MW, evaporate the volatile fractions and mix the resulting solution with the spent precipitation bath with subsequent distillation of water to contain her in crystallohydra e MMO 13.3%.

cl

4,149 hours

The invention relates to the production of chemical fibers, filaments and films, in particular to preparation in P (5con from solutions of cellulose in a direct solvent H-methylmorpholine-b oxide (MMO) by wet and dry-cure molding.

The aim of the invention is to increase the yield of the target product.

Example 1, When obtained - 1 ton of fiber, a spinning solution containing 1 ton of ci -cellulose, 7.3 t of SHO and 1.7 t of water5 enters the circulating precipitating bath of 50% SHO and 50% of water, V of precipitating In the plastic bath or in the first washing solution 5 containing 10%, 2.92 g of MMO also accumulate. During the final washing of the fiber, the wash water passes 1 j, .46 t M-U and the concentration I is set to IMO 0.25%,

The second wash water in the amount of 584 m is directed to the extraction of I-IMO by sorption on cation exchanger .-- 8 in the H-form Purified wash water is used in a new fiber washing cycle. Desorbts for I-MO from cation exchanger is carried out with water-isopropanol solution of ammonia containing 1 May, h

NH

3 ma.ch, N „0. May 16, h, isoproe -J l-iel4- and h 3 o J

Alcohol from the resulting solution is distilled ammonia-alcohol mixture with a portion of water, which is used in subsequent cycles of desorption No. 10 "Formed while 2.43 g of 60% aqueous solution of 2iO mixed with 5j84 tons of precipitation bath and 29.2 tons of the first The mortar or plastification bath is sent to the IMMO crystallization combined with distillation. The crystallization is carried out at 70 ° C, while 29.05 tons of water is distilled off and 8.42% of crystalline product containing 86g7% MMO is distilled. B, water (in terms of M Yu - 7.3 tons). The obtained crystalline hydrate MCO isg; it is used to prepare a dosing solution. After desorption, MMO cation resin is treated with n, sulfuric acid solution to convert to the H-form. The resulting acidic solution of ammonium sulfate is neutralized with ammonia. The resulting aqueous solution of sulfate and ammonia in an amount t with a concentration of (NH4) aS04 14, 8% is directed

.one

0

to a spray dryer to obtain marketable s-juny sulphate,

Pip Pi mep 2, In a precipitation bath, 3.65 tons of MMO accumulate, in a plasticizing 2.92 tons of MMO, and in the second wash water, 0.73 tons of MMO. The concentration of MMO in a plasticization bath is 5%,

A plasticizing bath in the amount of 58.4 tons is mixed with 292 tons (MMO concentration - 0525%) of the second wash water and is sent to extract MMOs by sorption on cation exchanger in the H-form. MMO desorption with ka-; thionite is carried out with a water-alcohol solution of ammonia containing 1 May, h, NH, 3 wt. h. and 16 May “h, isopropyl alcohol”. From the resulting solution, the ammonia-alcohol mixture is distilled off with a part of water. The resulting 60% aqueous solution of MMO in the amount of 6.08 t is mixed with 7.3 tons of sludge bath and They are found on thr1-1. The LEMOsIZATION IMO, combined with the distillation of water. The crystallization is carried out at 70 ° C. at the same time 4.96 tons of water is distilled off and Sj42 of crystalline product containing 86.7% MMO and 13 eZ% zod (7.3 tons, calculated as MMO) is obtained. preparation of the dope. After desorption, 1-5MO catconite is treated with ZjS n „-sulfuric acid solution for conversion into the H-form. The resulting acid, ammonium sulfate ammonium solution is neutralized with ammonia. This produces 15.87 tons of an aqueous solution of ammonium sulfate with the concentration (NH) SO, 14.8% which is sent to a sintering tailpipe to obtain commercial sulfate -monies

EXAMPLE 3 The recovery of IMO is carried out analogously to Example 1, but the solution for desorption of MMO from cationite contains 1 wt.h ,, NHj 4 wt.h, and 15 wt.h. isopropyl alcohol,

EXAMPLE 4, the recovery of IMO is carried out analogously to Example 2, but the solution for desorption of MMO from cationic acid sod, er; kit 1 wt. H KHj, 5 may h, HjO and 14 isopropyl alcohol,

EXAMPLE 5 Regeneration of MMO is carried out similarly to npHiviapy 2, but the E plasticizing bath accumulates 2.3 tons of MMO, and during the second wash

This is 1.35 tons of IMO. The concentration of IMO in the solution subjected to ion exchange is 0.62%.

 The invention allows fully (100%) regenerated methylmorpholine oxide in the form of a crystalline hydrate containing 13.3% of water, which makes it possible to use the product obtained directly in the preparation of the pr - di solution. In a known method, the amount of the regenerated product does not exceed 80% of the initial content in the spin solution, and the crystalline hydrate obtained contains 28% water, which requires additional dehydration to a water content of 13.3%.

Claims (1)

Invention Formula The method of regeneration of N-methylmorpholine-N-oxide from technological plants five 0 thieves in the manufacture of hydrated cellulose fibers, including mixing the spent process solutions, distilling water to isolate N-methylmorpholine-K-oxide crystalline hydrate and returning it to the preparation of the spinning solution, in order to increase the yield of the desired product, 0.25-0.62% solution of M-methylmorpholine-N-oxide is passed through a cation resin, from which a solution of ammonia in a mixture of water and isopropyl alcohol: sa with a mass ratio of ammonia, water and alcohol 1: 3-5: 14- 16 extract methylmorpholine-H- ksid, volatile fractions were distilled off and the resulting solution is mixed with the spent hydrochloric osaditel- bath and distillation was carried out to a water content of 13.3% in the crystalline hydrate.