The Spanish government, which has branded Catalonia’s quest to be made independent illegal, is determined to block the ballot on Sunday.
Last week Spanish national police stormed Catalan government offices and arrested officials backing the referendum.
But the clampdown may have backfired and instead fuelled support for the independence movement from moderate Catalans.
One Catalan said the sight of police storming government buildings convinced him that the region needs to be an independent state.
Jordi Herrera, on the sidelines of a rally on Friday, told the FT: “I was never sure we needed to be independent until then.
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“It made me so angry. I realised that Spain really owns us and can do what they like with us.”
Leading up to the referendum Spanish authorities have made several arrests, confiscated ballot boxes, taken back powers over public finances and cordoned off schools that might be used as polling stations.
One senior official in Madrid said: “We have to uphold the rule of law.
“But we know it could add to future problems in Catalonia if we allow this false narrative of oppression to take hold.”
Spanish state police are set to flood the streets this weekend in a last attempt to stop the poll.
But even if Madrid succeeds in disrupting the ballot they have failed to convince many Catalans that the region remain part of Spain.
Arthur Mas, the former president of Catalonia, said: “Using force to prevent what is a peaceful democratic vote is only going to add to the number of Catalan people who want to see an independent state.”
And in rallies across the northeastern region, the rhetoric is becoming more and more extreme.
Separatists have compared Madrid’s attempt to block the vote with dictator Francisco Franco’s brutal crackdown on Catalan language, culture and autonomy.
Jordi Sanchez, a leading pro-independence activists, told a rally in Barcelona: “Francoism is coming back to Spain.”
Catalonia is home to 7.5 million people and has its own devolved government, language and culture.
The region has insisted its wealthy areas support the rest of Spain during economic crises.
Spanish Prime Minister Mariano Rajoy has stated the vote on Sunday will be stopped.
He told Catalans: “If someone is asked to go to a polling station, do not go, because there can be no referendum and it would be an absolutely illegal act.”
But on Friday, Catalan leader Carles Puigdemont told Reuters the poll would go ahead, with no last minute compromise.
He said: “Everything is prepared at the more than 2,000 voting points so they have ballot boxes and voting slips, and have everything people need to express their opinion.”
Catalan independence supporters spent last night in schools, planning to stay for the whole weekend to keep the buildings open as polling stations for voters.