DE1211922C2 - Aid for filler retention in papermaking - Google Patents

Description

The present invention is the use of products by implementation from 0.8 to 0.95 mol of epichlorohydrin or α-dichlorohydrin with 1 mol of a di- or polyamine, its Amino groups are separated by at least 3 carbon atoms, in a diluent, preferably in water, as an aid for filler retention in papermaking.

As di- or polyamines on which the reaction products to be used according to the invention are based are, for example, trimethylenediamine, tetramethylenediamine, hexamethylenediamine, 1,3-diaminobutane, 2-oxy-l, 3-diaminopropane, dipropylenetriamine, Dioxydipropylenetriamine of the formula

H ₂ N ■ CH ₂ CH (OH) CH ₂ NHCH ₂ CH (OH) CH ₂ NH ₂ ,

Tetrapropylene pentamine, N, N'-diaminopropyl-tetramethylene diamine the formula

H ₂ N- (CH ₂ ) 3 NH (CH ₂ ) ₄ NH (CH ₂ ) 3
1,6,11-triamino-n-undecane of the formula
H ₂ N (CH ₂ ) ₅ C- (CH ₂ ) ₅ NH ₂ ;

NH ₂

The reaction products which y, / -diaminopropylalkylamines of the formula have proven particularly useful

35

H ₂ NCH ₂

CH ₂ CH ₂ -N- CH ₂ CH ₂ CH ₀ NH,

2>

45

Alkyl

such as B. γ, y'-diaminopropyl-methylamine and γ, γ'- diaminopropyl-butylamine, are based.

For the preparation of the inventive products to be used it is advantageously followed in which the reaction is carried the reaction components in the yerdühnüngsmittel at tempera doors between 2NC and 70 ⁰ C. The concentration of the reactants is expediently between 20 and 60 percent by weight. It is advisable to start the reaction at a concentration of about 40% and, after reaching a viscosity of about 50 to 100 cP, to finish it by diluting with the solvent used at a concentration of 15 to 30%.

How large the deficit of epichlorohydrin or .alpha.-dichlorohydrin is to be selected depends on the type of amine under consideration, on the desired storage stability and viscosity of the solution to be used and on the desired level of retention effect. It should be noted that the retention effect increases with the increase in viscosity and that, in order to achieve a good retention effect, the viscosity of a 15% solution at least 10 cP ₂₅ O, the viscosity of a 25% solution at least 40 cP ₂₅ O and the viscosity of a 35% solution should be at least 16OcP ₂₅ O. Sufficient storage stability of the solutions containing the reaction products, ie storage stability which extends to at least 1 year at room temperature, is given if the product obtained from a sample of the aqueous solution upon addition of twice the amount of 50% Potassium hydroxide has precipitated, dissolves again in water within an hour. If one wishes to improve the storage stability, the amount of epichlorohydrin or .alpha.-dichlorohydrin should be kept as low as possible within the specified range; if one wishes to increase the viscosity, the amount of epichlorohydrin or .alpha.-dichlorohydrin should be kept as high as possible within the specified range.

The percentages given in the example below are percentages by weight, based on the solid substance contained in the paper stock.

example

A conventionally prepared paper pulp with a degree of grinding of 23 ° Schopper-Riegler is used 0.06% of one of the reaction products listed in the table below under 1 to 7, 20% titanium dioxide and 5% of a commercially available pink-red organic pigment. You then get an excellent one Filler retention.

The excellent effect of the reaction products according to the invention listed under 1 to 7 compared to the effect of the reaction products, for their preparation to 1 mole of di- or polyamine more than 1 mole of epichlorohydrin or α-dichlorohydrin was used, is from the table below evident:

Mole epi
chlorohydrin
to 1 mole
Amine »/ O titanium
dioxide in '
¹ paper Color desi paper 0.87 : -14.2; deep pink 0.94 14.0 deep pink 0.88! 13.6 deepfrösäfot 0.93 13.8 deep pink 0.85 13.5 deep pink 0.82 12.5 deep pink 0.83 ■ 12.4 ■ deep pink 3; oo 8 <0 ι black pink ■ ϊ; 60 \ 11.0 pale pink

γ, / -diaminopropylmethylamm

γ, / -diaminopprppylbutylamine

Dipropylenetriamine i ......

Dioxydipropylenetriamine

Ν, Ν'-dianiinoprbpyI-tetramethylenediamine

Tetrapropylene peritam

1,6,11-TriämihÖ-n-üridecan

γ, / -DiamiriÖpropylrriethylamin .........

Tetraethylene pentamine ...

The preparation of the reaction products to be used according to the invention is explained in more detail below with reference to the preparation of a reaction product from epichlorohydrin and γ, / -diaminopropyl-methylamine:

A solution of 145 g of γ, / -diaminoprqpylmethylamine (1 mol) in 362 ml of water is admixed with 80.5 g of epichlorohydrin (0.87 mol) over the course of 1 hour at 30 ° C., while stirring and with cooling. Then increasing the temperature of the reaction mixture within ¹ hour Ii at 40 ° C and the mixture is stirred at this temperature so long as it is increased until the viscosity to about 7OcP; this is the case after about 80 minutes. Then 145 ml of water are added to the reaction mixture; this reduces the viscosity to around 40 cP. The mixture is now heated at 40 ° C. until the viscosity of the solution has risen to about 120 cP. This viscosity is reached after about 2½ hours, calculated from the addition of the 145 ml of water, or after 4 hours, calculated from the end of the addition of the epichlorohydrin. Finally, 171 ml of water are added to the solution. The solution prepared in this way contains 25 "Ii of the reaction product of epichlorohydrin and 7, / - diaminopropyimethylamine and has a viscosity of 145 cP at 25 ° C.

A product with practically the same properties is obtained if instead of 0.87 mol of epichlorohydrin 0.9 mol of a-dichlorohydrin is used. The conversion product is formed slower in this case, but can if desired by the addition of potassium hydroxide or sodium hydroxide in amounts up to 0.9Mol substantially be accelerated.

Claims (1)

Claim: Use of products made by reacting 0.8 to 0.95 moles of epichlorohydrin or α-dichlorohydrin with 1 mole of a di- or polyamine, whose amino groups by at least 3 carbon atoms are separated in one Diluents, preferably in water, have been prepared as an aid to filler retention in papermaking. IO