FI85510C - Process for recovery of lower aliphatic acid - Google Patents

Process for recovery of lower aliphatic acid Download PDF

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Publication number
FI85510C
FI85510C FI902675A FI902675A FI85510C FI 85510 C FI85510 C FI 85510C FI 902675 A FI902675 A FI 902675A FI 902675 A FI902675 A FI 902675A FI 85510 C FI85510 C FI 85510C
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FI
Finland
Prior art keywords
weight
acid
formic acid
cellulose
meadow
Prior art date
Application number
FI902675A
Other languages
Finnish (fi)
Swedish (sv)
Other versions
FI902675A0 (en
FI85510B (en
FI902675A (en
Inventor
Tapio Mattila
Kari Saari
Antti Vuori
Original Assignee
Kemira Oy
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kemira Oy filed Critical Kemira Oy
Priority to FI902675A priority Critical patent/FI85510C/en
Publication of FI902675A0 publication Critical patent/FI902675A0/en
Priority to PCT/FI1991/000168 priority patent/WO1991018864A1/en
Priority to FR9106473A priority patent/FR2665193A1/en
Publication of FI902675A publication Critical patent/FI902675A/en
Application granted granted Critical
Publication of FI85510B publication Critical patent/FI85510B/en
Publication of FI85510C publication Critical patent/FI85510C/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • C07C51/445—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by steam distillation
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment

Description

1 855101 85510

Menetelmä alemman alifaattisen hapon ottamiseksi talteen -Förfarande för ätervinning av lägre alifatisk syra 5 Tämä keksintö kohdistuu menetelmään alemman alifaattisen hapon ottamiseksi talteen tällä orgaanisella hapolla suoritetun keiton sellusta.The present invention relates to a process for the recovery of a lower aliphatic acid from the pulp of a cooking process with this organic acid.

Muurahaishappoa on aikaisemmin otettu talteen muurahaisha-10 polla suoritetun sellukeittoprosessin sellusta pesemällä sellu vedellä ja ottamalla muurahaishappo talteen saadusta laimeasta muurahaishappovesiliuoksesta tislaamalla. Tämän menetelmän haittapuolena on paitsi laimean hapon väkevöinnin vaatima vaikea tislaus ja sen aiheuttama suuri kustannus 15 myös se, että selluun jää esteröitynyttä muurahaishappoa.Formic acid has previously been recovered from the pulp of a pulp cooking process performed with the formic acid-10 path by washing the pulp with water and recovering the formic acid from the resulting dilute aqueous formic acid solution by distillation. The disadvantages of this method are not only the difficult distillation required by the concentration of dilute acid and the high cost involved, but also the fact that esterified formic acid remains in the pulp.

Parhaimmillaankin selluun jää puhdasvesipesun jälkeen muurahaishappoa n. 3 paino-% sellusta, kun hyväksyttävä muura-haishappopitoisuus sellussa on 1-2 paino-% sellusta ja tälle tasolle pääseminen vaatii hyvin suuria pesuvesimääriä sel-20 lun määrään nähden.At best, about 3% by weight of formic acid remains in the pulp after washing with pure water, while the acceptable formic acid content of the pulp is 1-2% by weight of the pulp and reaching this level requires very large amounts of washing water relative to the amount of pulp.

Esillä olevan keksinnön tarkoituksena on poistaa tässä tunnetussa menetelmässä esiintyvät epäkohdat ja aikaansaada menetelmä alemman alifaattisen hapon ottamiseksi talteen 25 tällä orgaanisella hapolla suoritetun keiton selluloosasta niin, että hapon määrä sellussa saadaan hyväksyttävälle tasolle erittäin taloudellisesti ja ilman, että selluun jäisi mitään merkittäviä määriä esteröitynyttä muurahaishappoa.The object of the present invention is to obviate the disadvantages of this known process and to provide a process for recovering a lower aliphatic acid from cellulose by cooking with this organic acid so that the amount of acid in the pulp is brought to an acceptable level very economically and without any significant amounts of esterified formic acid.

3030

Keksinnön pääasialliset tunnusmerkit ilmenevät oheisista patenttivaatimuksista.The main features of the invention appear from the appended claims.

Keksinnön mukaisessa menetelmässä alempi alifaattinen happo, 35 kuten muurahaishappo poistetaan kahdessa vaiheessa, ensin tyhjöhaihdutuksella korotetussa lämpötilassa ja tämän jäi-O ' keen pesulla tai vesihöyrystrippauksella.In the process of the invention, the lower aliphatic acid, such as formic acid, is removed in two steps, first by vacuum evaporation at an elevated temperature and washing of this residue or steam stripping.

2 855102 85510

Vakuumihaihdutus suoritetaan edullisesti n. 70-100°C:ssa ja höyrystrippaus on edullista suorittaa 100-140°C;ssa, kaikkein edullisimmin 110-120°C:ssa.The vacuum evaporation is preferably carried out at about 70-100 ° C and the steam stripping is preferably carried out at 100-140 ° C, most preferably at 110-120 ° C.

5 Keksinnön mukaisen menetelmän ensimmäisessä vaiheessa eli vakuumihaihdutuksessa saadaan yli 90 paino-% haposta talteen väkevänä, suoraan happokiertoon kelpaavana happona. Kun sellua tämän jälkeen pestään tai vesihöyrystripataan, saadaan puhdasta sellua, joka sisältää sidottua happoa 1-2 10 paino-% sellusta laskettuna ja vapaata happoa alle 0,5 pai-no-% sellusta laskettuna.In the first step of the process according to the invention, i.e. vacuum evaporation, more than 90% by weight of the acid is recovered as a concentrated acid which is directly recyclable. When the pulp is then washed or steam-stripped, pure pulp is obtained which contains 1-2% by weight of bound acid based on the pulp and less than 0.5% by weight of free acid based on the pulp.

Keksinnön mukaisella menetelmällä voidaan käsitellä sellaisen sellukeittoprosessin sellua, jossa keitossa on käytetty 15 jotakin alempaa alifaattista happoa, kuten muurahaishappoa, etikkahappoa tai propionihappoa.The process according to the invention can be used to treat the pulp of a pulp cooking process in which a lower aliphatic acid, such as formic acid, acetic acid or propionic acid, has been used in the cooking.

Keksintöä selostetaan seuraavassa lähemmin esimerkkien avulla.The invention is described in more detail below by means of examples.

2020

Esimerkki 1Example 1

Pyöröhaihduttimeen panostettiin 63,2 g muurahaishapposellu-loosaa, jonka kuiva-ainepitoisuus oli 18,45 paino-% ja muurahaishappopitoisuus (vapaa + sidottu) n. 390 paino-% 25 kuiva-aineesta. Lämpötila nostettiin 70°C:een ja muurahaishappoa haihdutettiin 2 h ajan 14 mbaarin paineessa. Tuotteeksi saatiin 14,1 g muurahaishapposelluloosaa, jonka kuiva-ainepitoisuus oli 82,75 paino-% ja joka sisälsi 10,3 paino-% vapaata ja 9,5 paino-% sidottua muurahaishappoa 30 kuiva-aineen määrästä. Väkevää muurahaishappoa (89,7 paino-%) saatiin talteen 49,0 g.The rotary evaporator was charged with 63.2 g of formic acid cellulose with a dry matter content of 18.45% by weight and a formic acid content (free + bound) of about 390% by weight of the dry matter. The temperature was raised to 70 ° C and the formic acid was evaporated for 2 h at 14 mbar. The product obtained was 14.1 g of formic acid cellulose with a dry matter content of 82.75% by weight and containing 10.3% by weight of free and 9.5% by weight of bound formic acid in an amount of 30 dry matter. Concentrated formic acid (89.7% by weight) was recovered in 49.0 g.

Vakuumihaihdutettu muurahaishapposelluloosa panostettiin putkireaktoriin. Reaktorin lämpötila nostettiin 120°C:een, 35 minkä jälkeen siihen syötettiin 4 h ajan 50 ml/h vettä 120°C:n lämpötilassa olevan höyrystimen kautta. Tuotteeksi saatiin 23,0 g muurahaishapposelluloosaa, jonka kuiva-ainepitoisuus oli 50,8 paino-% ja joka sisälsi 0,25 paino-% 3 85510 vapaata sekä 1,58 paino-% sidottua muurahaishappoa kuiva-aineen määrästä. Laimeaa muurahaishappoa (n. 1 paino-%) saatiin talteen 180 g.Vacuum evaporated formic acid cellulose was charged to a tubular reactor. The temperature of the reactor was raised to 120 ° C, after which 50 ml / h of water was fed for 4 h via an evaporator at 120 ° C. The product obtained was 23.0 g of formic acid cellulose with a dry matter content of 50.8% by weight and containing 0.25% by weight of 3,85510 free and 1.58% by weight of bound formic acid in the dry matter. Dilute formic acid (ca. 1% by weight) was recovered 180 g.

5 Esimerkki 25 Example 2

Pyöröhaihduttimeen panostettiin 75,2 g propionihapposellu-loosaa, jonka kuiva-ainepitoisuus oli 19,97 paino-% ja propionihappopitoisuus (vapaa + sidottu) n. 400 paino-% kuiva-aineesta. Lämpötila nostettiin 70°C:een ja propioni-10 happoa haihdutettiin 2 h ajan 14 mbaarin paineessa. Tuotteeksi saatiin propionihapposelluloosaa, joka sisälsi 0,10 paino-% vapaata ja 0,11 paino-% sidottua propionihappoa kuiva-aineen määrästä. Propionihappoa saatiin talteen 59,4 g.75.2 g of propionic acid cellulose having a dry matter content of 19.97% by weight and a propionic acid content (free + bound) of about 400% by weight of dry matter were charged to a rotary evaporator. The temperature was raised to 70 ° C and the propionic acid was evaporated for 2 h at 14 mbar. The product was propionic acid cellulose containing 0.10% by weight of free and 0.11% by weight of bound propionic acid in the dry matter. 59.4 g of propionic acid were recovered.

1515

Vakuumihaihdutettu propionihapposelluloosa panostettiin putkireaktoriin. Reaktorin lämpötila nostettiin 120°C:een, minkä jälkeen siihen syötettiin 4 h ajan 50 ml/h vettä 120°C:n lämpötilassa olevan höyrystimen kautta. Tuotteeksi 20 saatiin propionihapposelluloosaa, joka sisälsi alle 0,001 paino-% vapaata ja 0,01 paino-% sidottua propionihappoa kuiva-aineen määrästä. Laimeaa propionihappoa saatiin talteen 135 g.Vacuum evaporated propionic acid cellulose was charged to a tubular reactor. The temperature of the reactor was raised to 120 ° C, after which 50 ml / h of water was fed to it for 4 h via an evaporator at 120 ° C. The product 20 was propionic acid cellulose containing less than 0.001% by weight of free and 0.01% by weight of bound propionic acid in the dry matter. 135 g of dilute propionic acid were recovered.

25 Esimerkki 325 Example 3

Pyöröhaihduttimeen panostettiin 131,1 g muurahaishapposellu-loosaa, jonka kuiva-ainepitoisuus oli 18,45 paino-% ja muurahaishappopitoisuus (vapaa + sidottu) n. 390 paino-% kuiva-aineesta. Lämpötila nostettiin 70°Cseen ja muurahais-30 happoa haihdutettiin 2 h ajan 14 mbaarin paineessa. Tuotteeksi saatiin 25,5 g muurahaishapposelluloosaa, jonka kuiva-ainepitoisuus oli 95,05 paino-% ja joka sisälsi 6,0 paino-% vapaata ja 10,1 paino-% sidottua muurahaishappoa kuiva-aineen määrästä. Väkevää muurahaishappoa (88,1 pai-35 no-%) saatiin talteen 103,5 g.131.1 g of formic acid cellulose with a dry matter content of 18.45% by weight and a formic acid content (free + bound) of about 390% by weight of dry matter were charged to a rotary evaporator. The temperature was raised to 70 ° C and the formic acid was evaporated for 2 h at 14 mbar. The product obtained is 25.5 g of formic acid cellulose with a dry matter content of 95.05% by weight and containing 6.0% by weight of free and 10.1% by weight of bound formic acid in the dry matter. Concentrated formic acid (88.1 wt% to 35% by weight) was recovered.

Vakuumihaihdutettu muurahaishapposelluloosa pestiin kahdesti kuumalla (n. 90-95°C) vedellä. Vettä käytettiin kummallakin 4 85510 pesukerralla n. 8-kertainen painomäärä muurahaishapposellu-loosan määrään verrattuna. Tuotteeksi saatiin 142,3 g muura-haishapposelluloosaa, jonka kuiva-ainepitoisuus oli 17,0 paino-% ja joka sisälsi 0,3 paino-% vapaata ja 2,4 paino-% 5 sidottua muurahaishappoa kuiva-aineen määrästä. Laimeaa muurahaishappoa (n. 1,2 paino-%) saatiin talteen 260 g.The vacuum evaporated formic acid cellulose was washed twice with hot (ca. 90-95 ° C) water. Water was used in each of the 4,85510 washes in an amount of about 8 times the weight of the formic acid cellulose. The product obtained was 142.3 g of formic acid cellulose with a dry matter content of 17.0% by weight and containing 0.3% by weight of free and 2.4% by weight of bound formic acid in the dry matter. Dilute formic acid (ca. 1.2% by weight) was recovered in 260 g.

T>T>

Claims (7)

1. Förfarande för ätervinning av en lägre alifatisk syra ur cellulosa frän ett kok utfört med denna organiska syra, kännetecknat av att cellulosa innehällande nämnda syra 5 vakuumlndunstas vld förhöjd temperatur och till slut tvättas den vakuumindunstade cellulosan med hett vatten eller strip-pas med änga.A process for recovering a lower aliphatic acid from a cellulose from a boil made with this organic acid, characterized in that the cellulose containing said acid vacuum is at the elevated temperature of the vacuum evaporated and finally the vacuum evaporated cellulose is washed with hot water or stripped with meadow. 2. Förfarande enligt patentkravet 1, kännetecknat av att 10 vakuumindunstningen utförs vid ca. 70 - 100°C.Process according to claim 1, characterized in that the vacuum evaporation is carried out at approx. 70 - 100 ° C. 3. Förfarande enligt patentkravet 1 eller 2, kännetecknat av att ängstrippningen utförs vid 100 - 140°C. 15Method according to claim 1 or 2, characterized in that the meadow stripping is carried out at 100 - 140 ° C. 15 4. Förfarande enligt patentkravet 3, kännetecknat av att ängstrippningen utförs vid 110 - 120°C.Method according to claim 3, characterized in that the meadow stripping is performed at 110-120 ° C. 5. Förfarande enligt nägot av de föregäende patentkraven, kännetecknat av att vakuumindustningen utförs vid 70°C vid 20 ett tryck pä ca. 14 mbar ett par timmars tid.Process according to any of the preceding claims, characterized in that the vacuum industry is carried out at 70 ° C at a pressure of approx. 14 mbar a couple of hours. 6. Förfarande enligt nägot av de föregäende patentkraven, kännetecknat av att ängsstrippningen utförs med änga av en temperatur pä 120°C ca. 4 timmar. 25Method according to any of the preceding claims, characterized in that the meadow stripping is carried out with a meadow temperature of 120 ° C approx. 4 hours. 25 7. Förfarande enligt nägot av de föregäende patentkraven, kännetecknat av att man vakuumindunstar och tvättar med hett vatten eller ängstrippar myrsyra- eller propionsyracellulo-sa. 30Process according to any of the preceding claims, characterized in that vacuum evaporation and washing with hot water or meadow strips formic acid or propionic acid cellulose. 30
FI902675A 1990-05-29 1990-05-29 Process for recovery of lower aliphatic acid FI85510C (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
FI902675A FI85510C (en) 1990-05-29 1990-05-29 Process for recovery of lower aliphatic acid
PCT/FI1991/000168 WO1991018864A1 (en) 1990-05-29 1991-05-28 Process for the recovery of a lower aliphatic acid
FR9106473A FR2665193A1 (en) 1990-05-29 1991-05-29 PROCESS FOR THE RECOVERY OF LOWER ALIPHATIC ACID FROM PULP.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI902675 1990-05-29
FI902675A FI85510C (en) 1990-05-29 1990-05-29 Process for recovery of lower aliphatic acid

Publications (4)

Publication Number Publication Date
FI902675A0 FI902675A0 (en) 1990-05-29
FI902675A FI902675A (en) 1991-11-30
FI85510B FI85510B (en) 1992-01-15
FI85510C true FI85510C (en) 1992-04-27

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FI902675A FI85510C (en) 1990-05-29 1990-05-29 Process for recovery of lower aliphatic acid

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FI (1) FI85510C (en)
FR (1) FR2665193A1 (en)
WO (1) WO1991018864A1 (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4228171C2 (en) * 1992-08-25 1995-06-14 Kaemmerer Projekt Agentur Gmbh Process for the production of cellulose
FI95159C (en) * 1994-02-11 1995-12-27 Valtion Teknillinen Method and apparatus for separating cellulosic fibers from lignin
DE19516151A1 (en) 1995-05-03 1996-11-07 Sven Siegle Process for the production of a pulp from cellulosic material, the pulp itself and its use
FI108233B (en) * 1997-08-22 2001-12-14 Chempolis Oy Procedure for recovery of formic acid
EA202092813A1 (en) * 2018-05-28 2021-02-18 Пирсон Кэпитал Инвайронментал (Бейдзин) Лимитед EFFECTIVE METHODS AND COMPOSITIONS FOR REMOVING PRODUCTS FROM PRE-TREATMENT WITH ORGANIC ACIDS OF PLANT MATERIALS

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI52367C (en) * 1976-04-20 1977-08-10 Rosenlew Ab Oy W Method for recovering sulfur compounds, volatile alcohols and turpentine or the like from pulping
WO1982001902A1 (en) * 1980-12-05 1982-06-10 Robert K Jordan A process for pulping wood and bark in formic acid
FI74498C (en) * 1984-12-07 1988-02-08 Suomen Sokeri Oy Process for the recovery of aliphatic acids from liquids from alkaline α cellulose boil.

Also Published As

Publication number Publication date
WO1991018864A1 (en) 1991-12-12
FI902675A0 (en) 1990-05-29
FR2665193A1 (en) 1992-01-31
FI85510B (en) 1992-01-15
FI902675A (en) 1991-11-30

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